Category: 110860-60-1

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 110860-60-1, name is Methyl 5-amino-1-methyl-1H-pyrazole-4-carboxylate, This compound has unique chemical properties. The synthetic route is as follows., Safety of Methyl 5-amino-1-methyl-1H-pyrazole-4-carboxylate

18.5 mL of acetic acid is added to 4.1 mL of concentrated sulfuric acid and, while stirring under cooling with ice, 3.85 g (12.1 mmol) of 40% nitrosylsulfuric acid is dropwise added thereto. To the resulting mixture is gradually added 1.71 g (11.0 mmol) of the intermediate (b) (internal temperature: O0C or less), followed by stirring for 2 hours at 0C. 150 mg of urea is added to this reaction solution, followed by stirring for further 15 minutes at O0C to thereby prepare a diazo solution A.

According to the analysis of related databases, 110860-60-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; FUJIFILM Corporation; WO2009/110643; (2009); A1;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 110860-60-1, name is Methyl 5-amino-1-methyl-1H-pyrazole-4-carboxylate, A new synthetic method of this compound is introduced below., SDS of cas: 110860-60-1

9.2 g of the intermediate (b) obtained in the above-described Synthesis Example 1-1 is dissolved in a mixed solution of 55 mL of acetic acid and 37 mL of propionic acid at room temperature. The resulting solution is cooled with ice to an internal temperature of -3C, and a 40% by weight solution of nitrosylsulfuric acid in sulfuric acid is dropwise added thereto over 10 minutes at an internal temperature of -3C to 4C. After stirring the mixture at an internal temperature of 4C for 1 hour, 0.2 g of urea is added thereto. Thereafter, the mixture is cooled to an internal temperature of-3C, followed by stirring for further 10 minutes to obtain a diazonium salt solution. Separately, 10 g of the intermediate (d) obtained in the above-described Synthesis Example 1-1 is completely dissolved in 150 mL of acetone, and the solution is cooled to an internal temperature of 17C and added to the above-described diazonium salt solution over 25 minutes at an internal temperature ranging from -3C to 3C. After completion of the addition, the mixture is stirred at 3C for 30 minutes, and the ice bath is removed to allow the temperature of the mixture to rise to room temperature over 30 minutes. After stirring the mixture at room temperature for 30 minutes, crystals obtained are collected by filtration, spray washed with 150 mL of acetone, then with 100 mL of water. Crystals obtained are suspended in 400 mL of water without drying, and a 8N potassium hydroxide aqueous solution is added thereto to adjust the pH to 5.7. After stirring the mixture at room temperature for 25 minutes, crystals obtained are collected by filtration, sufficiently spray washed with water. The thus-obtained crude pigment (1)-1 is dried at room temperature for 12 hours. The thus-obtained crude pigment (1-I) is suspended in a mixed solvent of 580 mL of acetone and 1160 mL of water, followed by stirring for 30 minutes under reflux. Thereafter, the mixture is cooled to room temperature over 10 minutes, followed by stirring at room temperature for 5 hours to obtain 17,6 g of beta-type crystal form azo pigment (1)-1 having the crystal form of the invention and represented by formula (1). Yield: 91.0% Visual observation of the thus-obtained beta-type crystal form azo pigment (1)-1 with a transmission microscope (manufactured by JEOL Ltd.; JEM-1010; electron microscope) reveals that the length of the long axis of primary particles is about 150 nm. When X-ray diffraction of the beta-type crystal form azo pigment (1)-1 is measured under the aforesaid conditions, characteristic X-ray peaks are shown at Bragg angles (2theta+/-0.2) of 7.0, 26.4, and 27.3. The X-ray diffraction pattern with characteristic Cu Kalpha line is shown in Fig. 10.

The synthetic route of 110860-60-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; FUJIFILM Corporation; EP2343343; (2011); A1;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 110860-60-1, name is Methyl 5-amino-1-methyl-1H-pyrazole-4-carboxylate, A new synthetic method of this compound is introduced below., SDS of cas: 110860-60-1

9.2 g of the intermediate (b) obtained in the above-described Synthesis Example 1-1 is dissolved in a mixed solution of 55 mL of acetic acid and 37 mL of propionic acid at room temperature. The resulting solution is cooled with ice to an internal temperature of -3C, and a 40% by weight solution of nitrosylsulfuric acid in sulfuric acid is dropwise added thereto over 10 minutes at an internal temperature of -3C to 4C. After stirring the mixture at an internal temperature of 4C for 1 hour, 0.2 g of urea is added thereto. Thereafter, the mixture is cooled to an internal temperature of-3C, followed by stirring for further 10 minutes to obtain a diazonium salt solution. Separately, 10 g of the intermediate (d) obtained in the above-described Synthesis Example 1-1 is completely dissolved in 150 mL of acetone, and the solution is cooled to an internal temperature of 17C and added to the above-described diazonium salt solution over 25 minutes at an internal temperature ranging from -3C to 3C. After completion of the addition, the mixture is stirred at 3C for 30 minutes, and the ice bath is removed to allow the temperature of the mixture to rise to room temperature over 30 minutes. After stirring the mixture at room temperature for 30 minutes, crystals obtained are collected by filtration, spray washed with 150 mL of acetone, then with 100 mL of water. Crystals obtained are suspended in 400 mL of water without drying, and a 8N potassium hydroxide aqueous solution is added thereto to adjust the pH to 5.7. After stirring the mixture at room temperature for 25 minutes, crystals obtained are collected by filtration, sufficiently spray washed with water. The thus-obtained crude pigment (1)-1 is dried at room temperature for 12 hours. The thus-obtained crude pigment (1-I) is suspended in a mixed solvent of 580 mL of acetone and 1160 mL of water, followed by stirring for 30 minutes under reflux. Thereafter, the mixture is cooled to room temperature over 10 minutes, followed by stirring at room temperature for 5 hours to obtain 17,6 g of beta-type crystal form azo pigment (1)-1 having the crystal form of the invention and represented by formula (1). Yield: 91.0% Visual observation of the thus-obtained beta-type crystal form azo pigment (1)-1 with a transmission microscope (manufactured by JEOL Ltd.; JEM-1010; electron microscope) reveals that the length of the long axis of primary particles is about 150 nm. When X-ray diffraction of the beta-type crystal form azo pigment (1)-1 is measured under the aforesaid conditions, characteristic X-ray peaks are shown at Bragg angles (2theta+/-0.2) of 7.0, 26.4, and 27.3. The X-ray diffraction pattern with characteristic Cu Kalpha line is shown in Fig. 10.

The synthetic route of 110860-60-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; FUJIFILM Corporation; EP2343343; (2011); A1;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

Application of 110860-60-1, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 110860-60-1, name is Methyl 5-amino-1-methyl-1H-pyrazole-4-carboxylate belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

(11) Synthesis of azo pigment (2a) 9.2 g of the intermediate (b) is dissolved in a mixed solution of 55 mL of acetic acid and 37 mL of propionic acid at room temperature. The mixture is cooled with ice to an internal temperature of -3C, and a 40% by weight solution of nitrosylsulfuric acid in sulfuric acid is dropwise added thereto at an internal temperature of from -3C to 4C in 10 minutes. After stirring for 1 hour at an internal temperature of 4C, 0.2 g of urea is added thereto, followed by cooling to an internal temperature of -3C and further stirring for 10 minutes to obtain a diazonium salt solution. Separately, 10 g of the intermediate (d’) is completely dissolved in 150 mL of acetone, and cooled to an internal temperature of 17C, and then added to the above-described diazonium salt solution in 25 minutes at an internal temperature in the range of from-3C to 3C. After completion of the addition, the reaction solution is stirred for 30 minutes at 3C, and the ice bath is removed to allow the internal temperature to rise to room temperature. After stirring the reaction solution at room temperature for 30 minutes, precipitated crystals are collected by filtration, spray washed with 150 mL of acetone, then further spray washed with 100 mL of water. Crystals thus-obtained are suspended in 400 mL of water without drying, and an 8N potassium hydroxide aqueous solution is added thereto to adjust the pH to 5.7. After stirring at room temperature for 20 minutes, resulting crystals are collected by filtration, sufficiently spray washed with water, and then spray washed with 80 mL of acetone. The thus-obtained crystals are dried at room temperature for 12 hours. The thus-obtained crystals are suspended in 580 mL of acetone, and then the mixture is stirred for 30 minutes under reflux. Thereafter, the mixture is cooled to room temperature in 10 minutes, and formed crystals are collected by filtration, and dried at room temperature for 5 hours to obtain 17.1 g of the azo pigment (2a). Yield: 88.5%. Visual observation of the thus-obtained azo pigment (2a) under a transmission microscope (manufactured by JEOL Ltd.; JEM-1010 electron microscope) reveals that the length of the long axis of primary particles is about 15 mum. When X-ray diffraction of the azo pigment (2a) is measured under the aforesaid conditions, characteristic X-ray peaks are shown at Bragg angles (2theta+/-0.2) of 7.6 and 25.6. The X-ray diffraction pattern with characteristic Cu Kalpha line is shown in Fig. 1.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, Methyl 5-amino-1-methyl-1H-pyrazole-4-carboxylate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; FUJIFILM Corporation; EP2474575; (2012); A1;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 110860-60-1, name is Methyl 5-amino-1-methyl-1H-pyrazole-4-carboxylate, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of Methyl 5-amino-1-methyl-1H-pyrazole-4-carboxylate

[Example 4] 5.0 Parts of (Pig-9) synthesized according to Example 2 was added to 70.0 parts of a solvent having the same composition as the azo compound solution in the step (b) of Example 2 and stirred at 20C. Even by stirring for 1 hour, (Pig-9) was not completely dissolved but partially remained undissolved. At this time, a 92 mass% portion of (Pig-9) was dissolved in the solvent. This suspension was added to the poor solvent by the same method as in the step (c) of Example 2 and subsequently, the produced powder was treated in the same manner to obtain 4.8 parts (yield: 96.0%) of (Pig-9). The obtained pigment powder was observed with an eye through a transmission microscope (Electron Microscope JEM-1010, manufactured by JEOL Ltd.), as a result, the length in the long axis direction of the primary particle was 600 nm.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 110860-60-1.

Reference:
Patent; FUJIFILM Corporation; EP2474574; (2012); A1;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 110860-60-1, name is Methyl 5-amino-1-methyl-1H-pyrazole-4-carboxylate, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 110860-60-1

18.5 mL of acetic acid is added to 4.1 mL of concentrated sulfuric acid and, while stirring under cooling with ice, 3.85 g (12.1 mmol) of 40% nitrosylsulfuric acid is dropwise added thereto. To the resulting mixture is gradually added 1.71 g (11.0 mmol) of the intermediate (b) (internal temperature: O0C or less), followed by stirring for 2 hours at 0C. 150 mg of urea is added to this reaction solution, followed by stirring for further 15 minutes at O0C to thereby prepare a diazo solution A.

According to the analysis of related databases, 110860-60-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; FUJIFILM Corporation; WO2009/110643; (2009); A1;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

Some common heterocyclic compound, 110860-60-1, name is Methyl 5-amino-1-methyl-1H-pyrazole-4-carboxylate, molecular formula is C6H9N3O2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. SDS of cas: 110860-60-1

Synthesis of D-77; 1 g of compound (18) is added to 10 ml of phosphoric acid, and the mixture is heated to 30C to dissolve. This solution is cooled with ice and, while keeping the temperature of the solution at -5 to 0C, 0.46 g of sodium nitrite is added thereto, followed by stirring for 1 hour to obtain a diazonium salt solution. Separately, 0.93 g of the compound (17) is dissolved in 10 ml of methanol, and the aforesaid diazonium salt solution is added thereto at 8C or lower. At the time of completion of the addition, the ice bath is removed, followed by stirring the mixture for 2 hours. The reaction solution is added to 30 ml of acetonitrile, and the mixture is stirred at room temperature for 30 minutes. Crystals precipitated are collected by filtration, and spray-washed with 20 ml of acetonitrile. The crystals are added, without drying, to 50 ml of a 1% sodium hydrogencarbonate aqueous solution, and the mixture is stirred for 1 hour. The crystals are collected by filtration, and spray-washed with a sufficient amount of water. The thus-obtained crystals are added, without drying, to a solution composed of 15 ml of dimethylacetamide (DMAc) and 25 ml of water and, after stirring at 80C for 1 hour, the mixture is stirred at room temperature for 2 hours. Crystals precipitated are collected by filtration and spray-washed with 30 ml of a mixture of DMAc/water (=1/2). The thus-obtained crystals are dried to obtain 1.1 g of compound D-77 of the invention. Yield: 55.0%. Infrared absorption chart of compound D-77 is shown in Fig. 27. IR charts of typical compounds synthesized in Synthesis Examples 1 to 8 and those synthesized in the similar manner are shown in Figs. 1 to 27.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 110860-60-1, its application will become more common.

Reference:
Patent; FUJIFILM Corporation; EP2253674; (2010); A1;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

Related Products of 110860-60-1, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 110860-60-1, name is Methyl 5-amino-1-methyl-1H-pyrazole-4-carboxylate belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

(5) Synthesis of alpha-Type Crystal Morphology Azo Pigment Compound (2) (9.2 g) was dissolved in a mixed solution of 55 mL of acetic acid and 37 mL of propionic acid at room temperature, and the resulting solution was ice-cooled to lower the internal temperature to -3 C. A 40 mass % sulfuric acid solution of nitrosylsulfuric acid was added dropwise at an internal temperature of -3 C. to 4 C. over 10 minutes and after stirring at an internal temperature of 4 C. for 1 hour, 0.2 g of urea was added. Thereafter, the internal temperature was lowered to -3 C., and the mixture was further stirred for 10 minutes to obtain a diazonium salt solution. Separately, 10 g of Compound (3) was completely dissolved in 150 mL of acetone. This solution was cooled to an internal temperature of 17 C. and then added to the diazonium salt solution obtained above, at an internal temperature of -3 C. to 3 C. over 25 minutes. After the completion of addition, the mixture was stirred at 3 C. for 30 minutes, and the ice bath was removed. The temperature was raised to room temperature over 30 minutes, and the resulting solution was stirred at room temperature for 30 minutes. The obtained crystal was collected by filtration, spray-washed with 150 mL of acetone and further spray-washed with 100 mL of water. The obtained crystal was without drying suspended in 400 mL of water, and an aqueous 8 N potassium hydroxide solution was added to adjust the pH to 5.7. The system was stirred at room temperature for 20 minutes, and the obtained crystal was separated by filtration, thoroughly spray-washed with water and spray-washed with 80 mL of acetone. The obtained crystal was dried at room temperature for 12 hours.Crystal 1 obtained was suspended in 580 mL of acetone, and the suspension was stirred under reflux for 30 minutes and then cooled to room temperature over 10 minutes. The obtained crystal was separated by filtration and dried at 60 C. for 5 hours to obtain 17.1 g of an azo pigment composition containing an azo pigment represented by formula (1) having the crystal form of the present invention. Yield: 88.5%. The particle size of the obtained azo pigment was measured with an eye by using a transmission microscope (electron microscope JEM-1010, manufactured by JEOL Ltd.), as a result, the length in the long axis direction of the primary particle was about 15 mum.The obtained crystal was an alpha-type crystal morphology azo pigment shown in FIG. 1 or a tautomer thereof, having characteristic X-ray diffraction peaks at Bragg angles (2theta+/-0.2) of 7.6, 25.6 and 27.7 in the CuKalpha characteristic X-ray diffraction but not having a peak at 7.0 and 6.4 (alpha-Type Crystal Morphology Azo Pigment Composition 1).

The synthetic route of Methyl 5-amino-1-methyl-1H-pyrazole-4-carboxylate has been constantly updated, and we look forward to future research findings.

Related Products of 110860-60-1, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 110860-60-1, name is Methyl 5-amino-1-methyl-1H-pyrazole-4-carboxylate belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

(5) Synthesis of alpha-Type Crystal Morphology Azo Pigment Compound (2) (9.2 g) was dissolved in a mixed solution of 55 mL of acetic acid and 37 mL of propionic acid at room temperature, and the resulting solution was ice-cooled to lower the internal temperature to -3 C. A 40 mass % sulfuric acid solution of nitrosylsulfuric acid was added dropwise at an internal temperature of -3 C. to 4 C. over 10 minutes and after stirring at an internal temperature of 4 C. for 1 hour, 0.2 g of urea was added. Thereafter, the internal temperature was lowered to -3 C., and the mixture was further stirred for 10 minutes to obtain a diazonium salt solution. Separately, 10 g of Compound (3) was completely dissolved in 150 mL of acetone. This solution was cooled to an internal temperature of 17 C. and then added to the diazonium salt solution obtained above, at an internal temperature of -3 C. to 3 C. over 25 minutes. After the completion of addition, the mixture was stirred at 3 C. for 30 minutes, and the ice bath was removed. The temperature was raised to room temperature over 30 minutes, and the resulting solution was stirred at room temperature for 30 minutes. The obtained crystal was collected by filtration, spray-washed with 150 mL of acetone and further spray-washed with 100 mL of water. The obtained crystal was without drying suspended in 400 mL of water, and an aqueous 8 N potassium hydroxide solution was added to adjust the pH to 5.7. The system was stirred at room temperature for 20 minutes, and the obtained crystal was separated by filtration, thoroughly spray-washed with water and spray-washed with 80 mL of acetone. The obtained crystal was dried at room temperature for 12 hours.Crystal 1 obtained was suspended in 580 mL of acetone, and the suspension was stirred under reflux for 30 minutes and then cooled to room temperature over 10 minutes. The obtained crystal was separated by filtration and dried at 60 C. for 5 hours to obtain 17.1 g of an azo pigment composition containing an azo pigment represented by formula (1) having the crystal form of the present invention. Yield: 88.5%. The particle size of the obtained azo pigment was measured with an eye by using a transmission microscope (electron microscope JEM-1010, manufactured by JEOL Ltd.), as a result, the length in the long axis direction of the primary particle was about 15 mum.The obtained crystal was an alpha-type crystal morphology azo pigment shown in FIG. 1 or a tautomer thereof, having characteristic X-ray diffraction peaks at Bragg angles (2theta+/-0.2) of 7.6, 25.6 and 27.7 in the CuKalpha characteristic X-ray diffraction but not having a peak at 7.0 and 6.4 (alpha-Type Crystal Morphology Azo Pigment Composition 1).

The synthetic route of Methyl 5-amino-1-methyl-1H-pyrazole-4-carboxylate has been constantly updated, and we look forward to future research findings.

Related Products of 110860-60-1,Some common heterocyclic compound, 110860-60-1, name is Methyl 5-amino-1-methyl-1H-pyrazole-4-carboxylate, molecular formula is C6H9N3O2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

[Example 6] Production of (Pig-8): 6.8 Parts of the compound represented by formula (6) was added to a mixed solvent consisting of 28.7 parts of acetic acid, 5.1 parts of propionic acid and 1.8 parts of water and dissolved. This solution was ice-cooled to 5C, and 13.1 parts of 43% nitrosylsulfuric acid solution was added. During the addition, the temperature of the system climbed to 25C. After the addition of nitrosylsulfuric acid, a diazotization reaction was performed at 25C. After stirring for 1.5 hours, the reaction solution was cooled to 15C, and the excess nitrosylsulfuric acid was deactivated with urea to obtain a diazonium compound liquid preparation (step (a)). A solution obtained by adding and completely dissolving 7.4 parts of the compound represented by the following formula (9) in a mixed solution of 64.9 parts of acetic acid and 37.1 parts of sulfuric acid was prepared, and this solution was added to the diazonium compound liquid preparation above at 20C or less. After the completion of addition, the reaction was allowed to proceed at 20C for 1 hour to obtain an azo compound solution. During the reaction, precipitation of the pigment was not observed (that is, this solution was in a state of the obtained azo compound being completely dissolved) (step (b)). A poor solvent consisting of 210 parts of methanol and 30 parts of water was prepared and stirred at 15C and 250 rpm. In this poor solvent, the azo compound solution above was added dropwise (step (c)). After stirring as-is for 5 minutes, 292 parts of water was added and the produced powder was separated by filtration. The powder was added to 270 parts of water, and the excess acid was neutralized with aqueous ammonia. Filtration and water washing were again performed to obtain 12.5 parts (yield: 89.0%) of (Pig-8). The obtained pigment powder was observed with an eye through a transmission microscope (Electron Microscope JEM-1010, manufactured by JEOL Ltd.), as a result, the length in the long axis direction of the primary particle was 130 nm. Fig. 3 shows the IR spectrum of Pig-8.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Methyl 5-amino-1-methyl-1H-pyrazole-4-carboxylate, its application will become more common.