Day: February 22, 2021

Electric Literature of 138786-86-4, The chemical industry reduces the impact on the environment during synthesis 138786-86-4, name is Methyl 4-nitro-1H-pyrazole-3-carboxylate, I believe this compound will play a more active role in future production and life.

Example 12 Benzyl-(2S)-4-(5-{[(4-amino-1-phenyl-1H-pyrazol-3-yl)amino]carbonyl}pyridin-2-yl)-2-methylpiperazine-1-carboxylate A solution of methyl 4-nitro-1H-pyrazole-3-carboxylate (54.0 g, 315.6 mmol), phenylboronic acid (77.0 g, 631.2 mmol), copper(II) acetate (86.0 g, 473.4 mmol) and pyridine (49.9 g, 631.2 mmol) in methylene chloride (600 mL) was stirred at ambient temperature open to air for 48 hours. The reaction was evaporated in vacuo, diluted with 1 L of methylene chloride and filtered through a large plug of silica (washing with 2 L methylene chloride). The solvent was evaporated in vacuo to give methyl 4-nitro-1-phenyl-1H-pyrazole-3-carboxylate confirmed by 1H NMR (CDCl3) delta 8.61 (s, 1H), 7.73 (m, 2H), 7.50 (m, 3H), 4.02 (s, 3H).

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 4-nitro-1H-pyrazole-3-carboxylate, other downstream synthetic routes, hurry up and to see.

20154-03-4, name is 3-(Trifluoromethyl)-1H-pyrazole, 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. Safety of 3-(Trifluoromethyl)-1H-pyrazole

1,4-Diazabicyclo[2.2.2]octane (5.44 g, 48.5 mmol) and dimethylsulfamoyl chloride (4.76 mL, 44.46 mmol) were added to a solution of 3-(trifluoromethyl)pyrazole (5.5 g, 40.42 mmol) in acetonitrile (50 mL) at 0¡ã C. The mixture was allowed to warm to room temperature and stirred for 18 hours. The mixture was concentrated in vacuo and the residue was diluted with water. The product was extracted with AcOEt. The organic layer was separated, dried (MgSO4), filtered and the solvents evaporated in vacuo. The crude product was purified by flash column chromatography (silica gel; DCM). The desired fractions were collected and concentrated in vacuo to yield intermediate 43 (9.4 g, 95percent yield) as a colourless oil.

The synthetic route of 20154-03-4 has been constantly updated, and we look forward to future research findings.

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. 15878-00-9, name is 4-Chloro-1H-pyrazole, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 15878-00-9

Example 94 trans-2′-tert-Butyl-4-chloro-2’H-[1,3′]bipyrazolyl-4′-carboxylic acid (5-acetylamino-adamantan-2-yl)-amide Sodium hydride (60% in oil; 220 mg, 5.5 mmol) was added slowly to a solution of 4-chloro-pyrazole (710 mg, 6.9 mmol) in dry DMF (40 mL) at 0 C. in an ice-water bath. The mixture was stirred under argon for 10 minutes and the mixture was then heated to 40 C. for 2 hrs. trans-1-tert-Butyl-5-chloro-1H-pyrazole-4-carboxylic acid (5-acetylamino-adamantan-2-yl)-amide (270 mg, 0.69 mmol) was added and the mixture was heated at 110 C. overnight for 2 days and then cooled. The solvent was removed in vacuo. The resulting mixture was diluted with water and extracted with ethyl acetate (2X). The organic layers were combined and dried with magnesium sulfate, filtered and concentrated in vacuo. The solid was slurried in ether and filtered and dried under high vacuum to afford trans-2′-tert-butyl-4-chloro-2’H-[1,3′]bipyrazolyl-4′-carboxylic acid (5-acetylamino-adamantan-2-yl)-amide as a white solid (237 mg, 74%); ES(+)-HRMS m/z calcd for C23H31ClN6O2 (M+H) 459.2270, found 459.2268.

According to the analysis of related databases, 15878-00-9, the application of this compound in the production field has become more and more popular.

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. 943541-20-6, name is 3-Chloro-6-(1-methyl-1H-pyrazol-4-yl)pyridazine, This compound has unique chemical properties. The synthetic route is as follows., Safety of 3-Chloro-6-(1-methyl-1H-pyrazol-4-yl)pyridazine

STEP 2: 6-fluoro-1-M-f6-M-methyl-1 H-Dyrazol-4-yl)Dyridazin-3-yl)DiDeridin-4- vDindoline To a mixture of 6-fluoro-1-(piperidin-4-yl)indoline (256 mg, 1 mmol), 3- chloro-6-(1-methyl-1 H-pyrazol-4-yl)pyridazine prepared as in STEP 1 above (194 mg, 1.0 mmol) in DMSO (3 mL) was added DIPEA (0.52 mL, 3 mmol). The resulting mixture was sealed and heated at 180C for 1 .5 h under microwave irradiation. The resulting mixture was poured into H20 (30 mL) and the aqueous layer was extracted with 30% CH2Cl2/Et20 (30 mL x 5). The combined organic layer was dried (Na2S04) and filtered. The solvent was removed and the resulting residue was purified by column using 90-100% EtOAc/hexane as the eluent to yield the title compound, 6-fluoro-1 -(1-(6-(1- methyl-1 H-pyrazol-4-yl)pyridazin-3-yl)piperidin-4-yl)indoline.

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 943541-20-6.

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.

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. 2075-46-9, name is 4-Nitro-1H-pyrazole, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 2075-46-9

Step 1: Preparation of 3-chloro-1H-pyrazol-4-amine hydrochloride Into a 2 L three-necked round bottom flask affixed with an overhead stirrer, a temperature probe, an addition funnel, and a nitrogen inlet were added ethanol (600 mL) and 4-nitro-1H-pyrazole (50.6 g, 447 mmol). To this solution was added, in one portion, conc. HCl (368 mL) (note: rapid exotherm from 15 C. to 39 C.) and the resulting mixture was purged with nitrogen for 5 minutes. Palladium on alumina (5% w/w) (2.6 g, Alfa, black solid) was added to the mixture and stirred at room temperature while triethylsilane (208 g, 1789 mmol) was added drop-wise over 4 h. The reaction, which started to slowly exotherm from 35 C. to 55 C. over 2.0 h, was stirred for a total of 16 h and vacuum filtered through a plug of Celite to give a biphasic mixture. The mixture was transferred to a separatory funnel, the bottom aqueous layer was collected and rotary evaporated (60 C., 50 mmHg) to dryness with the aid of acetonitrile (3*350 mL). The resulting yellow solid was suspended in acetonitrile (150 mL) and allowed to stand for 2 h at room temperature followed by 1 h at 0 C. in the refrigerator. The solids were filtered and washed with acetonitrile (100 mL) to afford the titled compound 3-chloro-1H-pyrazol-4-amine hydrochloride (84 g, 97% yield, 80% purity) as a white solid: mp 190-193 C.; 1H NMR (400 MHz, DMSO-d6) delta 10.46-10.24 (bs, 2H), 8.03 (s, 0.54H), 7.75 (s, 0.46H), 5.95 (bs, 1H)); 13C-NMR (101 MHz, DMSO) delta 128.24, 125.97, 116.71.

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 2075-46-9.

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. 84547-61-5, name is (1-Methyl-1H-pyrazol-5-yl)methanol belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below. Quality Control of (1-Methyl-1H-pyrazol-5-yl)methanol

A solution of (1 -methyl- lH-pyrazol-5-yl)methanol (1.2 g, 10.71 mmol) in dichloromethane (25 mL) was treated with thionyl chloride (1.9 mL) at room temperature for 2 hours. Then the reaction was quenched by the addition of water (20 mL) and neutralized with saturated aqueous sodium carbonate. The organic layer was separated and the aqueous layer extracted with dichloromethane (3 x 20 mL). The combined organic layer was dried over by anhydrous sodium sulfate. The solids were filtered out and the filtrates were concentrated under reduced pressure to afford 5-(chloromethyl)-l -methyl-lH-pyrazole as light yellow oil (800 mg, 57 %). (ES, m/z): [M+H]+ 131.0 *H NMR (300 MHz, CDC13) delta 7.41 (d, 7 = 1.8 Hz, 1H), 6.27 (d, 7 = 1.8 Hz, 1H), 4.61 (s, 2H), 3.93 (s, 3H)

The synthetic route of 84547-61-5 has been constantly updated, and we look forward to future research findings.

Application of 1904-31-0, The chemical industry reduces the impact on the environment during synthesis 1904-31-0, name is 1-Methyl-1H-pyrazol-3-amine, I believe this compound will play a more active role in future production and life.

The compound N-methyl-3-aminopyrazole (2000 g, 20.6 mol, 1.0 eq) was dissolved in 6000 ml of concentrated hydrochloric acidAnd 2000 ml of water,Cooled to 0-5 C in an ice-salt bath,Then, 3.5 L of a saturated aqueous sodium nitrite solution (NaNO2, 2842.8 g, 41.2 mol, 2.0 eq) was added dropwise,After mechanical stirring reaction for 20 min,The reaction solution was added dropwise to an aqueous solution of 8000 ml of potassium iodide (8549.0 g, 51.5 mol, 2.5 eq) at 0 C,After completion of the dropwise addition,The reaction was allowed to spontaneously rise to room temperature for 4 h,After TLC detection reaction was complete,Add ethyl acetate extraction 2 times,The organic phase was dried with saturated brine and concentrated,The crude product was purified via flash column to give compound 3-iodo-l-methyl-lH-pyrazole (3473.8 g, 16.7 mol)Yield 81.0%.

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-Methyl-1H-pyrazol-3-amine, other downstream synthetic routes, hurry up and to see.

Electric Literature of 89088-55-1, A common heterocyclic compound, 89088-55-1, name is 5-Bromo-1-methyl-1H-pyrazol-3-amine, molecular formula is C4H6BrN3, 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.

As shown in step 3-iv of Scheme 3, compound 1010 (4.0 g, 22.7 mmol) was suspended in 100 mL of dry DCM along with carbonyl diimidazole (CDI, 3.69 g, 22.7 mmol) and reaction was refluxed under a nitrogen atmosphere for 3.0 hours. The reaction mixture was concentrated to a minimum volume under reduced pressure and an equal volume of hexanes was added to produce a sticky granular white precipitate. The solid was collected by filtration and washed with additional DCM/hexanes (1:1) to provide N-(5-bromo-1-methyl-1H-pyrazol-3-yl)-1H-imidazole-1-carboxamide (compound 1011, 1.11 g) as a fine granular ppt. This material was used directly in the subsequent reaction as is.

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.

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. 35344-95-7, name is 1H-Pyrazole-4-carbaldehyde, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 35344-95-7

into a 100-mL round-bottom flask, was placed a solution of tert-butyl N-[3- (methanesulfonyloxy)cyclobutyl]carbamate (2.65 g, 9.99 mmol, 1.00 eq.), lH-pyrazole-4- carbaldehyde (1.152 g, 11.99 mmol, 1.20 eq.) and Cs2C03 (6.52 g, 20.01 mmol, 2.00 eq.) in DMF (20 mL). The resulting solution was stirred for 4 h at room temperature. The reaction was then quenched by the addition of 100 mL of water. The resulting solution was extracted with 3×100 mL of ethyl acetate and the organic layers combined. The resulting mixture was washed with 100 mL of brine. The mixture was dried over anhydrous sodium sulfate and concentrated under vacuum. The crude product was purified by Flash-Prep-HPLC with the following conditions (CombiFlash-1): Column, CI 8 silica gel; mobile phase, MeCN/H2O=60:40 increasing to MeCN/H2O=70:30 within 3 min; Detector, UV 254 nm. The crude product was purified by Prep-SFC with the following conditions (prep SFC 350-2): Column: Phenomenex Lux 5u Cellulose-4 250*50mm; mobile Phase A: CO2:70, Mobile Phase B: MeOH-HPLC:30; Flow rate: 150 mL/min; 254 nm; RTL4.53; RT2:5.36. This resulted in 712 mg (54%) of tert-butyl N-[cw-3-(4-formyl-lH-pyrazol-l-yl)cyclobutyl]carbamate as a white solid.

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 35344-95-7.