Category: 5203-77-0

Application of 5203-77-0, 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. 5203-77-0, name is 1,3-Dimethyl-1H-pyrazol-5-ol belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

2.5 g (0.022 mol) of 1,3-dimethyl-5-hydroxypyrazole,40 mL of tetrahydrofuran was added to a three-necked flask,9.0 g of triethylamine (0.09 mol) was added with stirring.Ice bath control temperature of 5-10 ,A solution of 6.3 g (0.022 mol) of a solution of 2-methanesulfonyl-4-trifluoromethylbenzoyl chloride in tetrahydrofuran was added dropwise,Control the reaction temperature does not exceed 15 ,Drop finished,Remove the ice bath,The reaction was stirred at room temperature for 30 min,TLC detection reaction (ethyl acetate: petroleum ether = 4: 1, GF254, UV color)After the reaction is complete,2-methyl-2-hydroxypropanenitrile (0.2 g)Stirring slowly warming to 45-50 C reaction,TLC detection reaction (ethyl acetate: petroleum ether = 2: 1, GF254, UV color)After the reaction is complete,A solution of 5.5 g (0.023 mol) of tetrahydrofuran in 4-allyl-2-methoxyphenoxyacetyl chloride was added dropwise at room temperature,Control the temperature does not exceed 35 ,Drop at room temperature stirring 8hr,Add 50 mL of water to stir the crystals. The precipitated solid was collected by filtration and washed with 30% ethanol to give the title compound (7.2 g), yield: 57.8%

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, 1,3-Dimethyl-1H-pyrazol-5-ol, other downstream synthetic routes, hurry up and to see.

These common heterocyclic compound, 5203-77-0, name is 1,3-Dimethyl-1H-pyrazol-5-ol, its 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. COA of Formula: C5H8N2O

3-(2-Methoxyethoxy)-2-methyl-4-(methylsulfonyl)benzoic acid (1 g) was dissolved in chloroform (20 mL), and oxalyl chloride (500 mg) was added. A catalytic amount of dimethylformamide was added, followed by stirring at room temperature for 3 hours. Then, the solvent was distilled off under reduced pressure. The obtained residue was dissolved in tetrahydrofuran (5 mL), and then a solution having 5-hydroxy-1 ,3-dimethylpyrazole (450 mg) dissolved in tetrahydrofuran (15 mL) was slowly added. Triethylamine (0.65 mL) was added, followed by heating and refluxing for 5 hours. After completion of the reaction, the reaction mixture was cooled to room temperature and poured into water, then acidified with dilute hydrochloric acid and then extracted with ethyl acetate. The organic layer was washed with a saturated sodium chloride aqueous solution and then dried over magnesium sulfate. The solvent was distilled off under reduced pressure. The obtained residue was dissolved in acetonitrile (20 mL), and under cooling in an ice bath, triethylamine (0.65 mL) and acetone cyanohydrin (100 mg) were added, followed by stirring at room temperature for 18 hours. The reaction solution was poured into water and washed with a small amount of ethyl acetate. Then, the aqueous layer was acidified with dilute hydrochloric acid. It was extracted with ethyl acetate, and then, the organic layer was washed with a saturated sodium chloride aqueous solution and then dried over magnesium sulfate. The solvent was distilled off 5 under reduced pressure. The obtained residue was purified by column chromatography (developing solvent: ethyl acetate) to obtain 5-hydroxy-1 ,3-dimethylpyrazol-4-yl 3-(2- methoxyethoxy)-2-methyl-4-(methylsulfonyl)phenyl ketone (500 mg, the following Compound No. 5- 2) as slightly yellow solid.

The synthetic route of 1,3-Dimethyl-1H-pyrazol-5-ol has been constantly updated, and we look forward to future research findings.

Application of 5203-77-0, 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. 5203-77-0, name is 1,3-Dimethyl-1H-pyrazol-5-ol belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

2.5 g (0.022 mol) of 1,3-dimethyl-5-hydroxypyrazole,40 mL of tetrahydrofuran was added to a three-necked flask,9.0 g of triethylamine (0.09 mol) was added with stirring.Ice bath control temperature of 5-10 ,A solution of 6.3 g (0.022 mol) of a solution of 2-methanesulfonyl-4-trifluoromethylbenzoyl chloride in tetrahydrofuran was added dropwise,Control the reaction temperature does not exceed 15 ,Drop finished,Remove the ice bath,The reaction was stirred at room temperature for 30 min,TLC detection reaction (ethyl acetate: petroleum ether = 4: 1, GF254, UV color)After the reaction is complete,2-methyl-2-hydroxypropanenitrile (0.2 g)Stirring slowly warming to 45-50 C reaction,TLC detection reaction (ethyl acetate: petroleum ether = 2: 1, GF254, UV color)After the reaction is complete,A solution of 5.5 g (0.023 mol) of tetrahydrofuran in 4-allyl-2-methoxyphenoxyacetyl chloride was added dropwise at room temperature,Control the temperature does not exceed 35 ,Drop at room temperature stirring 8hr,Add 50 mL of water to stir the crystals. The precipitated solid was collected by filtration and washed with 30% ethanol to give the title compound (7.2 g), yield: 57.8%

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, 1,3-Dimethyl-1H-pyrazol-5-ol, other downstream synthetic routes, hurry up and to see.

Synthetic Route of 5203-77-0,Some common heterocyclic compound, 5203-77-0, name is 1,3-Dimethyl-1H-pyrazol-5-ol, molecular formula is C5H8N2O, 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.

Weigh 1.7g (0.015mol) 1,3- dimethyl-5-pyrazolone-ol in 250mLthree-necked flask was added 50mL1,2-Dichloroethane was dissolved and weighed 4.0g (0.040mol) oftriethylamine in the system. Under ice cooling, Intermediate (a-2) of1,2-dichloroethane solution (0.010mol (a-2)) was addeddropwise to the system, during the addition using argon. After the reaction 1hThe reaction was followed by HPLC, the reaction was completefeed reaction solution containing intermediate (a-3) a. Counter-containingintermediate (a-3) ofLiquid should be supplemented with 1.0g (0.010mol) oftriethylamine and several drops of acetone cyanohydrin, temperature controlledat 50 ~ 60 and argon gas protectionProtection, response 2h, HPLC trace reaction. Aftercompletion of the reaction was added 100mL of water was slowly added dropwiseHCl, stirring at room temperature, until pH = 3about. 200mL extract was washed with water to remove theaqueous layer, the organic layer was washed twice, dried over anhydrous sodiumsulfate, the organic solvent was removed by rotary evaporation,To give 3.6g a tan solid, a powdered compound a.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,3-Dimethyl-1H-pyrazol-5-ol, its application will become more common.

Synthetic Route of 5203-77-0, 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. 5203-77-0, name is 1,3-Dimethyl-1H-pyrazol-5-ol belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

200 mg (0.71 mmol) of 2-methyl-3-methylsulfonyl-4-trifluoromethylbenzoic acid together with 87 mg (0.78 mmol) of 5-hydroxy-1,3-dimethylpyrazole and a catalytic amount of 4-N,N-dimethylaminopyridine were initially charged in 20 ml of dry CH2Cl2, and 163 mg (0.85 mmol) of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride were added. The mixture was stirred at RT for 3 h, and 3 ml of 1 M HCl were then added. After phase separation, the aqueous phase was extracted with CH2Cl2. The organic phases were dried and concentrated. The residue was taken up in 20 ml of acetonitrile and 143 mg (1.42 mmol) of triethylamine, and eight drops of acetone cyanohydrine and a spatula tip of KCN were added. The mixture was stirred at RT for 16 h and concentrated. 15 ml of CH2Cl2 and then 2 ml of 1M HCl were added to the residue. After phase separation, the aqueous phase was extracted with CH2Cl2. The combined organic phases were dried and concentrated. The residue was purified chromatographically. What was isolated were 112.7 mg of pure product.

The synthetic route of 1,3-Dimethyl-1H-pyrazol-5-ol has been constantly updated, and we look forward to future research findings.

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. 5203-77-0, name is 1,3-Dimethyl-1H-pyrazol-5-ol belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below. name: 1,3-Dimethyl-1H-pyrazol-5-ol

At room temperature, 1,3-dimethyl-1H-pyrazole-5-ol (1.12 g, 0.01 mol) and (1.58 g, 0.02 mol) pyridine were sequentially dissolved in 20 ml of dichloromethane. The low temperature bath was cooled to 0 C. To the above mixture was added dropwise a solution of 3,7-dichloroquinoline-8-acyl chloride (2.73 g, 0.0105 mol) in dichloromethane (10 ml),The dropping rate was 5 drops / 30 seconds. After the addition was complete, the mixture naturally rose to room temperature and reacted for 4 hours. To the reaction mixture was added 10 ml of a saturated aqueous sodium hydrogen carbonate solution, and the mixture was extracted with dichloromethane (3 * 15 ml). The organic layers were combined,Wash with water (1 * 15ml), saturated brine, and dry over anhydrous magnesium sulfate. desolvate under reduced pressure to obtain 2.52 g of product with a yield of 75%

The synthetic route of 5203-77-0 has been constantly updated, and we look forward to future research findings.

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. 5203-77-0, name is 1,3-Dimethyl-1H-pyrazol-5-ol, A new synthetic method of this compound is introduced below., category: pyrazoles-derivatives

2.5 g (0.022 mol) of 1,3-dimethyl-5-hydroxypyrazole,Toluene 30mL into the three bottles,9.0 g of triethylamine (0.09 mol) was added with stirring.Ice bath control temperature of 5-10 ,A toluene solution of 6.3 g (0.022 mol) of 2-methanesulfonyl-4-trifluoromethylbenzoyl chloride was added dropwise,Control the reaction temperature does not exceed 15 ,Drop finished,Remove the ice bath,The reaction was stirred at room temperature for 30 min,TLC detection reaction (ethyl acetate: petroleum ether = 4: 1, GF254, UV color)After the reaction is complete,2-methyl-2-hydroxypropanenitrile (0.2 g)Stirring slowly warming to 45-50 C reaction,TLC detection reaction (ethyl acetate: petroleum ether = 2: 1, GF254, UV color)After the reaction is complete,Was added 9.0 g (0.023 mol) of N-ethanesulfonyl-N- (4-trifluoromethoxyphenyl) bromoacetamide,Control temperature 60-65 C Reaction 8hr,After completion of the reaction, the mixture was cooled and added with 50 mL of water.The organic layer was separated and washed with saturated brine. The solvent was recovered to dryness and the residue was separated by column chromatography to give 7.1 g of the desired product, 48.1%

The synthetic route of 5203-77-0 has been constantly updated, and we look forward to future research findings.

Electric Literature of 5203-77-0, 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. 5203-77-0, name is 1,3-Dimethyl-1H-pyrazol-5-ol belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

Intermediate 9 (4 mmol), dissolved in dry dichloromethane( 60 mL), and DCC (4.8 mmol) were mixed together and stirred at room temperature for 1 h. Then 1,3-dimethyl-1H-pyrazol-5-ol (4 mmol) and DMAP (0.4 mmol) were added to the above solution,and stirred for a further 24-36 h at room temperature. After adding dichloromethane (30 mL), the resultant mixture was washed sequentially with 2 N hydrochloric acid (100 mL), saturated NaHCO3 and saturated brine and dried over anhydrous sodium sulfate.The residue solution was evaporated in vacuum and purified by silica gel column chromatography using gradient elution of ethyl acetate/hexane (V/V = 1/2) to obtain the desired intermediate 10.

The synthetic route of 1,3-Dimethyl-1H-pyrazol-5-ol has been constantly updated, and we look forward to future research findings.

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 5203-77-0 as follows. Application In Synthesis of 1,3-Dimethyl-1H-pyrazol-5-ol

a. 1.22 g (10.9 mmol) of 1,3-dimethyl-5-hydroxypyrazole and 1.1 g (10.9 mmol) of triethylamine are dissolved in 75 ml of acetonitrile and treated at 0 C. with 3.5 g (10.9 mmol) of 2-chloro-4-methylsulfonyl-3-(oxazol-5-yl)-benzoyl chloride in 50 ml of acetonitrile. Stirring is continued at 0 C for 1 hour, and 4.45 g (44 mmol) of triethylamine and 0.61 g (7.2 mmol) of acetocyanohydrin are subsequently added dropwise at room temperature. The solution is stirred at room temperature for 12 hours. For working up, the mixture is first treated with dilute hydrochloric acid and extracted using methyl tert-butyl ether. The ether phase is then extracted using 5% strength potassium carbonate solution. After the aqueous phase has been acidified with hydrochloric acid, the product is extracted from the aqueous phase using ethyl acetate. The ethyl acetate phase is dried using sodium sulfate and concentrated. This gives 1.2 g of crude product which is purified by column chromatography. This gives 0.4 g (27% of theory) of 1,3-dimethyl-4-[2-chloro-4-methylsulfonyl-3-(oxazol-5-yl)-benzoyl]-5-hydroxy-pyrazole, m.p.: 236-241 C. The compound shown in the table which follows is obtained by a similar method:

According to the analysis of related databases, 5203-77-0, the application of this compound in the production field has become more and more popular.

Synthetic Route of 5203-77-0, 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. 5203-77-0, name is 1,3-Dimethyl-1H-pyrazol-5-ol, This compound has unique chemical properties. The synthetic route is as follows.

Step 6: Synthesis of 4-(4-chloro-3-ethylsulfinyl-2-methyl benzoyl)-5-hydroxy-1,3-dimethylpyrazole128 mg (1.14 mmol) of 5-hydroxy-1,3-dimethylpyrazole were added to 270 mg (purity 95% by weight; 1.04 mmol) of 4-chloro-3-ethylsulfinyl-2-methylbenzoic acid in 20 ml of dichloromethane (CH2Cl2). 239 mg (1.24 mmol) of 1-(3′-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride were added, and the mixture was stirred at RT for 16 h. For work-up, 3 ml of 1M HCl were added, and the organic phase was freed from the solvent. 210 mg (2.07 mmol) of triethylamine, 10 drops of acetone cyanohydrin and a spatula tip of potassium cyanide were added to the residue in 20 ml of acetonitrile. The reaction mixture was stirred at RT for 16 h and then freed from the solvent. The residue was stirred at RT with 25 ml of a mixture of aqueous saturated sodium bicarbonate solution and diethyl ether for 10 min. The phases were separated, and the aqueous phase was acidified with dilute HCl and then extracted with CH2Cl2. The organic phase was freed from the solvent and the residue was then purified chromatographically. This gave 100 mg of clean product.

The chemical industry reduces the impact on the environment during synthesis 1,3-Dimethyl-1H-pyrazol-5-ol. I believe this compound will play a more active role in future production and life.