Day: March 18, 2021

These common heterocyclic compound, 120068-79-3, name is 5-Amino-1-(2,6-dichloro-4-(trifluoromethyl)phenyl)-1H-pyrazole-3-carbonitrile, 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. Formula: C11H5Cl2F3N4

EXAMPLE 3 Preparation of 5-Amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-3-cyanopyrazol-4-yl disulphide Acetonitrile (837 g) was added to a chlorobenzene solution (627.8 g) which contained 5-amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-3-cyanopyrazole (366.6 g, 1.14 mol). The mixture was heated at 50-64 C. under reduced pressure (0.5 atmosphere) and dried by the distillation of about 45 ml of the acetonitrile. After cooling to 18 C., sulphur monochloride (77 g, 0.57 mol) was added rapidly over 1 minute. The temperature of the mixture increased to 35 C. and was maintained at 35 C. by cooling until the exotherm ceased and for a further 0.3 hour. The mixture was then degassed (to remove hydrogen chloride) by heating at 40 C. under reduced pressure, and then heated at 80 C. for 1 hour at atmospheric pressure. After cooling to 30 C., ammonia was added to bring the pH to 6.5-7, cooled to 5 C. and the product filtered off, washed with chlorobenzene/acetonitrile and dried at 95 C. under vacuum to give the title compound (365.2 g) in typical yield of 89.4% and 98.4% purity.

The synthetic route of 5-Amino-1-(2,6-dichloro-4-(trifluoromethyl)phenyl)-1H-pyrazole-3-carbonitrile has been constantly updated, and we look forward to future research findings.

Reference of 25016-11-9, A common heterocyclic compound, 25016-11-9, name is 1-Methyl-1H-pyrazole-4-carbaldehyde, molecular formula is C5H6N2O, 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.

A mixture of the combined organic layer having 1-methyl-1H-pyrazole-4-carbaldehyde and ethyl acetate obtained from step 1, hydroxylamine hydrochloride (63.48 gm, 0.9135 moles) were refluxed at 70-80 C. for 2-4 hours. The progress of the reaction was monitored by HPLC. The reaction mixture was cooled to 0-5 C., to this added DM water (100 ml) and 25% aqueous ammonia solution (100 ml) at 0-5 C. The reaction mixture was stirred for 10 min at 20-30 C. The organic layer was separated and aqueous layer was extracted with ethyl acetate (250 ml). The entire organic layer was transferred to the reaction vessel and washed with 10% brine solution (500 ml). Stirred for 10 min and separated the final aqueous layer and organic layer. The organic layer was evaporated to obtain the 1-methyl-1H-pyrazole-4-carbaldehyde oxime.

The synthetic route of 25016-11-9 has been constantly updated, and we look forward to future research findings.

Synthetic Route of 5744-40-1, 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 5744-40-1 as follows.

A suspension of Step 1 intermediate (5.3 g, 31.52 mmol) in aqueous sodium hydroxide (5%, 32 mL) was refluxed for 4 h. The reaction mixture was cooled to 0 C and acidified with cone. HQ till pH 2-3. The precipitated solid was filtered and dried well to obtain 3.67 g of the desired product. lH NMR (300 MHz, CDC13): delta 3.87 (s, 3H), 4.13 (s, 3H), 6.61 (s, 1H), 6.71 (s, 1H).

According to the analysis of related databases, 5744-40-1, the application of this compound in the production field has become more and more popular.

Related Products of 14531-55-6, A common heterocyclic compound, 14531-55-6, name is 3,5-Dimethyl-4-nitro-1H-pyrazole, molecular formula is C5H7N3O2, 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.

Lambda -(1 -(2-Hydroxyethyl)-3,5-dimethyl-1 H-pyrazol-4-yl)-5-(m-tolyl)oxazole-4-carboxamideStep 1 : To a solution of 3,5-dimethyl-4-nitro-1 H-pyrazole (500 mg, 3.52 mmol) in MeCN (5 ml_), Cs2C03 (1.26 g, 3.87 mmol) and 2-bromoethanol (0.3 ml_, 4.21 mmol) was added. The resulting mixture was refluxed (90 C) for 3 h, then the reaction mixture was allowed to reach rt. The mixture was diluted with DCM, filtered, the filter cake rinsed with DCM and the filtrate concentrated in vacuo. The residue was partitionned between water and EtOAc, the org. layer was separated and the aq. layer was extracted with EtOAc (1x). The combined org. layers were washed with brine, dried (MgS04), filtered and concentrated in vacuo to yield 2- (3,5-dimethyl-4-nitro-1 H-pyrazol-1-yl)ethanol as a white solid. LC-MS conditions A: tR = 0.53 min, [M+H]+= 186.39

The synthetic route of 14531-55-6 has been constantly updated, and we look forward to future research findings.

Related Products of 52222-73-8, 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. 52222-73-8, name is 4-(Trifluoromethyl)-1H-pyrazole, This compound has unique chemical properties. The synthetic route is as follows.

3-(3-(4-(chloromethyl)benzyl)isoxazol-5-yl)pyridin-2 -amine (Intermediate B, 80mg, 0.27mmol) and 4-(trifluoromethyl)-lH-pyrazole (l45mg, l .07mmol) were dissolved in NMP (lml). Potassium 2- methylpropane-2-olate (1M in THF, 0.80mL, 0.80mmol) was added and the mixture was stirred for 5min at 60C. The cooled reaction mixture was directly purified by column chromatography (Si02, hexane/ethyl acetate). Fraction containing the product were concentrated under reduced pressure and further purified by HPLC to yield 3-(3-(4-((4-(trifluoromethyl)-lH-pyrazol-l-yl)methyl)benzyl)isoxazol- 5-yl)pyridin-2-amine (75mg, 0. l9mmol, 70%) as a white solid. 400 MHz ‘H NMR (CDC13) d 8.14 (d, ./ = 3.7 Hz, 1H), 7.73 (s, 1H), 7.69 (dd, J= 7.7, 1.8 Hz, 1H), 7.64 (s, 1H), 7.30 (d, J= 8.2 Hz, 2H), 7.22 (d, J = 8.2 Hz, 2H), 6.70 (dd, J= 7.7, 4.9 Hz, 1H), 6.25 (s, 1H), 5.43 (s, 2H), 5.29 (s, 2H), 4.05 (s, 2H). MS: 400.3 [M+H]+.

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

Synthetic Route of 79080-39-0, These common heterocyclic compound, 79080-39-0, name is 1-Methyl-1H-pyrazole-3-carbonitrile, 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.

To 1 -methyl-1 H-pyrazole-3-carbonitrile (2.7 g, 25.2 mmol) in Et20 (150 mL) cooled in ice bath was added LiAIH4 (27.7 mL, 55.5 mmol, 2M in THF) slowly, and the reaction mixture was allowed to warm to room temperature and stirred overnight. The reaction was then cooled in ice bath and quenched by sequential addition of water (4 mL), 15percentNaOH solution (4 mL), and water (12 mL). The mixture was then stirred for 15 minutes, and the resulting solid was filtered. The filtrate was dried over MgS04 and concentrated to afford (1 -methyl- 1 H-pyrazol-3-yl)methanamine (1 .28 g) as a clear oil. LC-MS (ES) m/z = 1 12 [M+H]+. 1H NMR (400 MHz, DMSO-c/6): delta 1 .69 (br. s, J = 1 .5 Hz, 2H), 3.60 (s, 2H), 3.75 (s, 3H), 6.12 (d, J = 2.0 Hz, 1 H), 7.53 (d, J = 2.0 Hz, 1 H).

Statistics shows that 1-Methyl-1H-pyrazole-3-carbonitrile is playing an increasingly important role. we look forward to future research findings about 79080-39-0.

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. 16617-46-2, name is 3-Amino-1H-pyrazole-4-carbonitrile, A new synthetic method of this compound is introduced below., COA of Formula: C4H4N4

Following the procedure described in Example 1 wherein propanol was used as the solvent instead of ethanol, 86percent of the product was obtained with m. p. 185-188 ¡ãC.

The synthetic route of 16617-46-2 has been constantly updated, and we look forward to future research findings.

Reference of 113100-53-1, A common heterocyclic compound, 113100-53-1, name is 1-Methyl-3-(trifluoromethyl)-1H-pyrazole-4-carboxylic acid, molecular formula is C6H5F3N2O2, 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.

To a solution of 1-methyl- 3-(trifluoromethyl)-1H-pyrazole-4-carboxylic acid (400 mg, 2.06 mmol) in THF (6 mL) was added BH3.DMS (0.412 mL, 4.12 mmol) dropwise over 1 mm at 0 C under nitrogen. Thereaction was stirred at 0 C for 0.5 h, at 20 C for 0.5 h, and at 80 C for 3 h. Then the reaction was quenched with MeOH (20 mL) at 0 C, and the mixture was concentrated under reduced pressure to give the title compound, which was used directly in the next step without further purification. MS (ESI) m/z: 181.0 [M+Hj 1H NMR (400MHz, DMSO-d6) 3 = 7.81 (s, 1H), 5.12 (t, J=S.3 Hz, 1H), 4.40 (d, J5.1 Hz, 2H), 3.88 (s, 3H).

The synthetic route of 113100-53-1 has been constantly updated, and we look forward to future research findings.

Adding a certain compound to certain chemical reactions, such as: 345637-71-0, name is 2-(5-Methyl-3-(trifluoromethyl)-1H-pyrazol-1-yl)acetic acid, 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 345637-71-0, Recommanded Product: 2-(5-Methyl-3-(trifluoromethyl)-1H-pyrazol-1-yl)acetic acid

Example 17 N-[5-({7-[(1R)-2-Hydroxy-1-methylethyl]-7H-pyrrolo[2,3-d]pyrimidin-5-yl}carbonyl)pyridin-3-yl]-2-[5-methyl-3-(trifluoromethyl)-1H-pyrazol-1-yl]acetamide (5-Methyl-3-trifluoromethyl-pyrazol-1-yl)acetic acid (46.8 mg, 0.225 mmol) was added to (R,S) (5-aminopyridin-3-yl){7-[(1R)-1-methyl-2-(tetrahydro-2H-pyran-2-yloxy)ethyl]-7H-pyrrolo[2,3-d]pyrimidin-5-yl}methanone (66 mg, 0.173 mmol) (see Preparation 36), 1-propylphosphonic acid cyclic anhydride (0.31 mL, 0.519 mmol) and DIPEA (0.09 mL, 0.606 mmol) in THF (5 mL). The mixture was heated at reflux for 48 hours, evaporated in vacuo and partitioned between saturated aqueous sodium bicarbonate (5 mL) and ethyl acetate (5 mL). The organic phase was dried over sodium sulfate, evaporated in vacuo and the residue was purified by column chromatography on silica gel (gradient of EtOAc:Hexane 85:15) to afford the intermediate as an off white solid in 53% yield, 52 mg. 10% Hydrochloric acid in 1,4-dioxane (0.4 mL) was added to the intermediate (52 mg, 0.091 mmol) in THF (2 mL) and the mixture was stirred at room temperature for 1.5 hours. The mixture was evaporated in vacuo and triturated with pentane:diethyl ether (3:1, 1 mL) to afford the title compound as an off white solid in 94% yield, 42 mg. 1H NMR (400 MHz, DMSO) delta: 1.49 (d, 3H), 2.32 (d, 3H), 3.56 (m, 1H), 5.00 (m, 1H), 5.20 (s, 2H), 6.56 (s, 1H), 8.45 (s, 1H), 8.54 (s, 1H), 8.79 (s, 1H), 9.02 (s, 2H), 9.48 (s, 1H), 11.05 (s, 1H); LCMS (system 4): Rt=2.86 min; m/z 488 [M+H]+.

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, 2-(5-Methyl-3-(trifluoromethyl)-1H-pyrazol-1-yl)acetic acid, other downstream synthetic routes, hurry up and to see.

Related Products of 132712-71-1, 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. 132712-71-1, name is 3-Methyl-1H-pyrazol-5-ol belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

To 300 ml of N, N-dimethylformamide was added 22 g of 3-methylpyrazol-5-ol followed by 14 g of anhydrous potassium carbonate and 29 g of 3-nitrobromobenzene, and the mixture was stirred under heating and refluxing for 2 hours and then cooled At room temperature, ethyl acetate and water were added slowly, and the mixture was extracted, dried, concentrated and the residue was subjected to silica gel column chromatography to obtain 21 g of 3-methyl-1- (3-nitrophenyl) alcohol.

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