Category: 141573-95-7

Reference of 141573-95-7, A common heterocyclic compound, 141573-95-7, name is Ethyl 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylate, molecular formula is C8H10F2N2O2, 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.

l,2,3,4-tetrahydro-9-isopropyl-l,4-methanonaphthalen-5-amine320 mg (1 eq. ; 9: 1 syn:anti mixture) in 2 ml THF and 325 mg (1.6 mmol)DFMMP (1) in 2 ml THF were added to a suspension of 268mg (1.5 eq.) KOtBu in 10 ml THF at 0C. After stirring at room temperature over night the reaction mixture was poured out in water and extracted twice with acetic ether. The purified organic extracts were washed with water and a saturated NaCl solution, dried, filtered and concentrated over sodium sulphate. The residue was filtrated through a silicagel column (Si02 ; hexane/acetic ether 1 : 1) and the desired product Isopyrazam was obtained in 77 % yield (440 mg) (purity GC 100 % ; HPLC – 254nm > 99 % as 86.5: 12.7 symanti mixture).

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

141573-95-7, name is Ethyl 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylate, belongs to pyrazoles-derivatives compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. SDS of cas: 141573-95-7

To the toluene layer was added 25% caustic soda solution159 g (0.994 mole) of the compound were added thereto, and the mixture was heated to 65 DEG C and stirred for 45 minutes. The aqueous layer was separated, and 54 g of water and 160.2 g (1.54 mole) of 35% hydrochloric acid were added to the toluene layer, followed by stirring at 85 for 15 minutes. After cooling to room temperature the resulting crystals were filtered, washed with 180 g of water and dried in vacuo at 60 & lt; RTI ID = 0.0 & gt;To obtain 155.8 g (yield 98%) of 3- (difluoromethyl) -1-methyl-1H-pyrazole-4-carboxylic acid.

The synthetic route of 141573-95-7 has been constantly updated, and we look forward to future research findings.

Adding a certain compound to certain chemical reactions, such as: 141573-95-7, name is Ethyl 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylate, belongs to pyrazoles-derivatives compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 141573-95-7, HPLC of Formula: C8H10F2N2O2

Example 9 (0339) (0340) At room temperature under a nitrogen atmosphere, 5.91 parts (purity: 95.9%, R isomers/S isomers=95.4/4.6) of (R)-1,1,3-trimethyl-4-aminoindane, 21.5 parts of tetrahydrofuran, and 1.29 parts (purity: 60%) of sodium hydride were mixed. The obtained mixture was heated and refluxed for 1 hour. The reaction liquid was cooled to room temperature. To the obtained solution was added dropwise a solution in which 6.13 parts (purity: 97.8%) of ethyl 1-methyl-3-difluoromethylpyrazole-4-carboxylate had been dissolved in 9.2 parts of tetrahydrofuran. The obtained mixture was heated in an oil bath at 90 C. and stirred for 8 hours while tetrahydrofuran was evaporated. At this time, tetrahydrofuran in the same amount of the evaporated tetrahydrofuran was added thereto freshly at times, such that the concentration of the reaction liquid became constant. The obtained mixture was cooled to room temperature and then 92.0 parts of toluene was added thereto. The obtained mixture was washed sequentially with 5% hydrochloric acid, a saturated sodium bicarbonate solution, and saturated physiological saline. The obtained organic layer was concentrated under reduced pressure to obtain 13.1 parts of (R)-(-)-N-(1,1,3-trimethylindan-4-yl)-1-methyl-3-difluoromethylpyrazole-4-carboxylic acid amide. The content of (R)-(-)-N-(1,1,3-trimethylindan-4-yl)-1-methyl-3-difluoromethylpyrazole-4-carboxylic acid amide was 64.8% (the yield with respect to ethyl 1-methyl-3-difluoromethylpyrazole-4-carboxylate of 86.4%). Further, the ratio of R isomers/S isomers of (R)-(-)-N-(1,1,3-trimethylindan-4-yl)-1-methyl-3-difluoromethylpyrazole-4-carboxylic acid amide was 95.4/4.6.

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, Ethyl 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylate, other downstream synthetic routes, hurry up and to see.

Application of 141573-95-7, 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 141573-95-7 as follows.

To a solution of 2.93 g (14.3 mmol, 1.00 eq) DFMMP and 3.00 g (17.3 mmol, 1.20 eq) 2-(bi(cyclopropan)-2-yl)benzenamine in 20 mL dry dioxane, 10.0 ml (72.2 mmol, 5.40 eq) triethylamine was added, followed by 7.20 g (57.1 mmol, 4.00 eq) A1C13 which was added in one portion. After stirring the reaction mixture for 1 h, it was cooled with ice and quenched with water. The aqueous phase was extracted twice with ethyl acetate, the combined organic layers were washed with water and brine, dried over Na2S04 and the solvent removed under reduced pressure. The crude product was purified by column chromatography (MTBEJ to yield (4.1 g, 85 %) Sedaxane. HPLC: t, = 10.9 min + 11.4 min (trans +cis 62:38); HPLC/MS: tr = 12.7 min [M+H]+ 332; tr = 13.3 min [M+H]+ 332; NMR (500 MHz, CDC13) delta (ppm) = 8.46 (s, br, 0.35H), 8.08 (s, br, 0.65H), 8.26 (d, 3J = 8.2 Hz, 0.35H), 8.07 (d, 3J = 8.1 Hz, 0.65H), 7.98 (d, 3J = 6.3 Hz, 1H), 7.27-7.20 (m, 1H), 7.09-7.04 (m, 2H), 7.02-6.80 (m, 1H), 3.95 (s, 1H), 3.94 (s, 2H), 1.98-1.93 (m, 0.35H), 1.66-1.62 (m, 0.65H), 1.17-1.13 (m, 0.65H), 1.07-1.02 (m, 0.35H), 0.97-0.87 (m, 1H), 0.80-077 (m, 1H), 0.71-0.67 (m, 0.65H), 0.42-0.38 (m, 1.35H), 0.30-0.25 (m. 0.35H), 0.21-0.11 (m, 1.65H), 0.07-0.01 (m, 1H).

According to the analysis of related databases, 141573-95-7, the application of this compound in the production field has become more and more popular.

Related Products of 141573-95-7, 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. 141573-95-7, name is Ethyl 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylate, This compound has unique chemical properties. The synthetic route is as follows.

Preparation Example V.13-difluoromethyl-1-methyl-1H-pyrazol-4-ylcarboxylic acidA mixture of ethyl 3-difluoromethyl-1-methyl-1H-pyrazol-4-ylcarboxylate (1.4 g, 52 mmol) and aqueous sodium hydroxide solution (10% strength, 3.1 g, 8 mmol) was stirred at 60 C. for 2 h. The reaction mixture was cooled to room temperature, and the pH was then adjusted to 1 using concentrated hydrochloric acid. The reaction mixture was cooled further to 0 C., resulting in the precipitation of a solid. The precipitated solid was filtered off, washed with cyclohexane and dried under reduced pressure. This gave 3-difluoromethyl-1-methyl-1H-pyrazol-4-ylcarboxylic acid as a solid (amount: 0.8 g; yield: 87%). 1H-NMR (DMSO-d6): delta=3.9 (s, 2H), 7.2 (t, 1H), 8.35 ppm (s, 1H).

The chemical industry reduces the impact on the environment during synthesis Ethyl 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylate. I believe this compound will play a more active role in future production and life.

These common heterocyclic compound, 141573-95-7, name is Ethyl 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylate, 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. Quality Control of Ethyl 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylate

In a 100 mL reaction flask, add 1-methyl-3-difluoromethyl-1H-pyrazole-4-carboxylic acid ethyl ester (38 mmol) represented by formula (II), and then add 10% by mass NaOH30mL of aqueous solution, heated to 60 C and stirred until the reaction solution was transparent, then naturally cooled to room temperature,Acid was added to the reaction solution to adjust the pH to about 2.0, and a solid was precipitated.After the filter residue is washed and dried,1-methyl-3-difluoromethyl-1H-pyrazole-4-carboxylic acid represented by the formula (III) was obtained.

The synthetic route of Ethyl 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylate 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. 141573-95-7, name is Ethyl 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylate, A new synthetic method of this compound is introduced below., Recommanded Product: Ethyl 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylate

In a three-necked round bottom flask, 186 g of 3-difluoromethyl-1-methyl-1H-pyrazole-4-carboxylic acid ethyl ester (VII) was added.(0.91 mol), 900 ml of ethanol, and a solution of sodium hydroxide 44 g, (1.1 mol) dissolved in 900 ml of water, heated to 50C to 80C, and incubated for 3 hours, the reaction of the starting material was complete by TLC, and the ethanol was concentrated under reduced pressure to remove ethanol Add 100ml of toluene to extract, recover toluene in organic phase, cool the water phase to room temperature, adjust the PH value to 1-2 with 31% hydrochloric acid, cool to about 10C for 0.5 hours, filter and dry to obtain product 3- (Difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid 6 (DFPA) 152 g, yield 95%.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Some common heterocyclic compound, 141573-95-7, name is Ethyl 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylate, molecular formula is C8H10F2N2O2, 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. category: pyrazoles-derivatives

3 -Difluoromethyl-1-methyl-1H-pyrazole-4-carboxylic acid ethyl ester (53.3 mg) was dissolved in liquid ammonia (10 mL). A column (500mm x 4.6mm i.d.) packed with aluminium oxide (4.501 g) was placed in the oven and the temperature was raised to 100C before pure liquid ammonia was pumped through. Then pure liquid ammonia was pumped through the system at 0.3 mLmin”1 and the pressure adjusted to 100 bar using an adjustable back pressure regulator.The system was left pumping pure liquid ammonia for 10 minutes then switched to the reaction solution at 0.3mL min^forSO min. At this time, pure liquid ammonia was pumped through the system for another 1 hour at 0.3mL min”1. All the reaction solution was collected as it exited the reaction column, at the end of the reaction, the ammonia was allowed to evaporate, the residue was dissolved in methanol and analysed by HPLC (87-91% conversion, 98.4% selectivity).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 141573-95-7, its application will become more common.

Adding some certain compound to certain chemical reactions, such as: 141573-95-7, name is Ethyl 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylate, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 141573-95-7. 141573-95-7

The compound of formula (III) was added to a 5% aqueous solution of sodium hydroxide, reacted at 60 C for 3 hours, and then hydrochloric acid was added to neutralize the pH to a weak acidity,(IV) 1-methyl-3-difluoromethyl-1H-pyrazole-4-carboxylic acid;The compound of formula (IV) (40 mmol) was refluxed with thionyl chloride (0.4 mol) for 4 hours and distilled under reduced pressure to give(V) 1-methyl-3-difluoromethyl-1H-pyrazole-4-carbonyl chloride;

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 Ethyl 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylate.

A common heterocyclic compound, 141573-95-7, name is Ethyl 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylate, molecular formula is C8H10F2N2O2, 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. 141573-95-7.

The azinium salt (10.0 g, 29.9 mmol) was suspended in 50 mL of toluene. A solution of NaOH (1.44 g, 36.0 mmol) in 50 mL of water was added and the biphasic mixture was heated to 60 C. for 3 h. The mixture was then cooled to rt, the phases split and the aqueous phase extracted with 20 mL of toluene. The combined org. phases were used in the next step without further purification. To the solution of the aminal in toluene were added ethyl alpha-ethoxymethylene-4,4-difluoro-3-oxobutyrate (6.64 g, 29.9 mmol) and p-TsOH monohydrate (0.57 g, 3.0 mmol). The solution was stirred overnight at rt, then heated to 60 C. for one hour. The solution was then cooled to it and extracted with 30 mL sat. NaHCO3 solution. The org. phase was used in the next step without further purification. To the org. phase was added 10% KOH solution (24.1 g). The biphasic mixture was heated to 60 C. and the disappearance of the ester monitored by GC. When the ester had completely vanished, the solution was cooled to rt. The phases were then split and the aqueous phase was heated to 55 C. Then, 30% H2SO4 solution (16 g) were added and stirring continued for 60 min. The solution was then cooled to 5 C. and the precipitated product removed by filtration. The precipitate was washed with cold water and dried under reduced pressure overnight (p<20 mbar, 50 C.). The product was obtained as a yellow powder (2.87 g, 16.3 mmol, 55% yield based on the azinium salt). 1H NMR (500 MHz, DMSO-d6): delta (ppm)=8.33 (s, 1H); 7.22 (t, J=54 Hz, 1H); 3.93 (s, 3H). 13C NMR (125 MHz, DMSO-d6): delta (ppm)=163.0; 145.1 (t, J=24 Hz); 136.1; 113.0 (t, J=3 Hz); 109.6 (t, J=234 Hz); 39.2. 19F NMR (470 MHz, DMSO-d6): delta (ppm)=-126.0 (d, J=54 Hz). mp=205 C. Purity (cal. HPLC): 97.1% (0.4% iso-DFP acid) The synthetic route of Ethyl 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylate has been constantly updated, and we look forward to future research findings.