Day: February 25, 2021

Reference of 578008-32-9, The chemical industry reduces the impact on the environment during synthesis 578008-32-9, name is tert-Butyl 3-amino-5-methyl-1H-pyrazole-1-carboxylate, I believe this compound will play a more active role in future production and life.

Example 13Preparation of 3-(4-fluorophenylsulfinyl)-N-( -methyl-lH-pyrazol-3- vDisoq uinolin- 1-amine[00258] A sealed tube was charged with Pd2(dibenzylideneacetone)3 (14 mg,0.016 mmol), 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (26 mg, 0.047 mmol), tert-butyl 3 -amino-5 -methyl- lH-pyrazole-l-carboxylate from Example 1 Step D (177 mg, 0.89 mmol), Na2C03 (1 10 mg, 1.04 mmol), l-bromo-3-(4- fluorophenylsulfinyl)isoquinoline from Example 10 Step D (260 mg, 0.74 mmol) and degassed toluene (5.2 mL), and then water (0.014 mL) was added with stirring. The sealed tube was heated in an oil bath at 100 C for 2 h, and then in a microwave synthesizer at 100 C for 1.5 h. The mixture was filtered and the filtrate was concentrated. The solid residue was triturated with MeOH and collected by filtration and dried under reduced pressure to afford tert-butyl 3-(3-(4- fluorophenylsulfinyl)isoquinolin- 1 -ylamino)-5 -methyl- 1 H-pyrazole- 1 -carboxylate (166 mg, 40 %) as a white solid. JH NMR (300 MHz, DMSO-t/6) delta 1.52 (s, 9H), 2.25 (s, 3H), 6.46 (s, 1H), 7.40 (t, 2H), 7.83-7.90 (m, 4H), 8.00-8.03 (m, 2H), 8.17 (d, 1H), 10.61 (s, 1H); LC-MS (ESI) m/z 467 (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, tert-Butyl 3-amino-5-methyl-1H-pyrazole-1-carboxylate, other downstream synthetic routes, hurry up and to see.

Adding a certain compound to certain chemical reactions, such as: 15366-34-4, name is Methyl 1H-pyrazole-3-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 15366-34-4, Recommanded Product: 15366-34-4

Methyl 1 H-pyrazole-3-carboxylate (12.61 mg, 0.1 mmol) was dissolved in a 0. 105M solution of potassium tert-butoxide in ethanol (1 ml, 11.78 mg, 0.105 mmol). After stirring at room temperature for 5 mins, a 0. 1 M solution of 4-bromo-2- (bromomethyl) phenyl phenylmethyl ether in ethanol (1 ml, 35.6 mg, 0.1 mmol) was added and the resulting solution was stirred and heated at 60C under nitrogen for 4hrs. After cooling the mixture was diluted with ethanol (1 ml) and a 0.5M solution of lithium hydroxide in water (1 ml, 11.97mg, 0. 5mmol) was added. The mixture was stirred overnight at 40C. After cooling 2M hydrochloric acid (0. 3moi, 0. 6mmol) was added and the mixture was diluted with water. Dichloromethane was added and the mixture stirred vigorously. The organic layer was separated and the solvent removed in vacuo. The residue was purified by mass directed autopurification to yield the title compound. 1-({5-bromo-2-[(phenylmethyl) oxy] phenyl} methyl)-5-methyl-1 H-pyrazole-3-carboxylic acid: (10. 7mg, 27.6%). ‘H NMR 8 : 5.08 (2H, s), 5.34 (2H, s), 6.72 (1H, d, J = 2.2Hz), 6.92 (1H, d, J = 8.8Hz), 7.23 (1H, d, J = 2Hz), 7.30-7. 39 (6H, m), 7.45 (1H, d, J = 2Hz). t = 3.38, [MH+] 387, 389 [MH-] 385,387.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Methyl 1H-pyrazole-3-carboxylate, and friends who are interested can also refer to it.

Adding a certain compound to certain chemical reactions, such as: 127107-23-7, name is 1-Methyl-1H-pyrazol-4-amine hydrochloride, 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 127107-23-7, Product Details of 127107-23-7

1. 5.0 kg of l-methyl-pyrazol-4-amine hydrochloride and 9.2 kg of water were added to a flask (“Flask 1”). 2. The contents of Flask 1 were stirred at 15-25 C until dissolved. 3. 9.6 kg of tert-butyl 4-(2-chloropyrimidin-4-yl)-2-methylbenzylcarbamate, 15.6 kg of 2-butanol, and 14.6 kg of water were added to a separate flask (“Flask 2”). 4. The contents of Flask 2 were stirred at 55-65 C until a clear solution was observed. 5. The contents of Flask 1 were added to Flask 2, rinsing Flask 1 with 5 kg of water and transferring the rinse to Flask 2. 6. The contents of Flask 2 were heated to 80-90 C and were stirred at 80-90 C for at least 16 hours. 7. The contents of Flask 2 were cooled to 30-40 C. 8. 46.1 g of water was added to Flask 2 while maintaining the temperature at 30-40 C. 9. 24.2 kg of ammonium hydroxide (28-30%) was diluted with 25.7 kg of water and added to Flask 2 over at least 1 hour. 10. 5 kg of water was added to Flask 2. 11. The contents of Flask 2 were cooled to 10-20 C over at least 1 hour. 12. The contents of Flask 2 were stirred at 10-20 C for at least 1 hour. 13. The contents of Flask 2 were vacuum filtered to isolate a solid product. 14. The product was dried under vacuum at < 75 C. 15. 7.65 kg of product was obtained (90.0% yield), and MR conformed to prior assignments. If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

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. 52222-73-8, name is 4-(Trifluoromethyl)-1H-pyrazole belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 52222-73-8

A mixture of compound 26 (200 mg, 0.342 mmol), 4-(trifluoromethyl)-1H-pyrazole (93 mg, 0.68 mmol), copper(I) iodide (13 mg, 0.068 mmol), 8-hydroxyquinoline (20 mg, 0.14 mmol), and potassium carbonate (95 mg, 0.68 mmol) in DMSO (2 mL) was stirred at 130 C under N2 atmosphere overnight. The mixture was quenched with saturated aqueous NH4Cl solution and the insoluble materials were removed by filtration. The filtrate was extracted with AcOEt. The organic layer was successively washed with water and brine, dried over MgSO4, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/AcOEt = 70:30 to 30:70) and crystallized from AcOEt-iPr2O to give the title compound as a pale yellow solid (80 mg, 0.13 mmol, 37%). MS (ESI/APCI) m/z 640.3 [M+H]+. 1H NMR (300 MHz, DMSO-d6) delta 1.96-2.10 (4H, m), 3.20 (2H, t, J = 8.2 Hz), 3.83 (2H, br s), 4.40 (2H, t, J = 8.1 Hz), 7.38-7.47 (2H, m), 7.48-7.57 (2H, m), 8.28 (1H, s), 9.05 (2H, s), 9.18 (1H, s), 10.02 (1H, s). 13C NMR (101 MHz, DMSO-d6) delta 18.0, 27.5, 30.3, 48.4, 52.0, 112.8 (t, J = 16.9 Hz), 113.1-113.4 (m), 113.8 (q, J = 37.4 Hz), 120.2, 122.7 (q, J = 266.3 Hz), 124.1, 125.6, 127.5, 128.9 (q, J = 3.7 Hz), 132.6 (t, J = 13.2 Hz), 134.3, 137.3, 138.5-138.6 (m), 140.7, 149.2, 156.7, 158.9 (dd, J = 253.5, 5.5 Hz), 171.1. Mp 242-245 C. Anal. Calcd for C26H19ClF5N7O3S: C, 48.79; H, 2.99; N, 15.32. Found: C, 48.82; H, 2.92; N, 15.06.

The synthetic route of 52222-73-8 has been constantly updated, and we look forward to future research findings.

Synthetic Route of 51105-90-9, 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 51105-90-9 as follows.

Potassium carbonate (822 mg, 5.95 mmol) was added to a solution of 2-(2-(benzyloxy)ethoxy)ethyl methanesulfonate (598 mg, 2.181 mmol) and methyl 1 H-pyrazole-4-carboxylate (250 mg, 1.982 mmol) in DMF (15 mE) and heated to 60 C. for 2 days. The reaction was cooled to it, diluted with EtOAc (50 mE) and washed sequentially with water (30 mE), sat. aq. NaHCO3 (30 mE) and 20% v/v brine (30 mE). The organic layer was dried (MgSO4) and concentrated in vacuo. The crude product was purified by chromatography on silica gel (12 g column, 0-100% EtOAc/ isohexane) to afford the sub-title compound (472 mg) as a colourless oil.?H NMR (400 MHz, DMSO-d6) oe 8.33 (d, 1H),7.87 (d, 1H), 7.38-7.30 (m, 2H), 7.30-7.24 (m, 3H), 4.44 (s,2H), 4.32 (t, 2H), 3.80 (t, 2H), 3.72 (s, 3H), 3.58-3.53 (m,2H), 3.53-3.48 (m, 2H).mlz 305.1 (M+H) (ES)

According to the analysis of related databases, 51105-90-9, the application of this compound in the production field has become more and more popular.

Electric Literature of 3469-69-0,Some common heterocyclic compound, 3469-69-0, name is 4-Iodopyrazole, molecular formula is C3H3IN2, 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.

4-Iodopyrazole (2 g, 10.311 mmol) was dissolved in DMF (50 mL), sodium hydride (1.25 g, 30.933 mmol) was added at 0 C, and the reaction was stirred for 30 min.Methyl iodide (1.3 mL, 20.622 mmol) was slowly added dropwise to the above solution, warmed to room temperature, and stirred for 22 hours.After the reaction was completed, filter, concentrate the filtrate, dilute with water, extract with ethyl acetate (80 mL ¡Á 3), collect the organic phase, dry over anhydrous sodium sulfate, filter, and concentrate the filtrate.Silica gel column chromatography was separated and purified (PE / EtOAc (v / v) = 18/1) to obtain 1.37 g of light yellow liquid, yield: 63.9%.

The synthetic route of 3469-69-0 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. 25016-20-0, name is 1-Methyl-1H-pyrazole-3-carboxylic acid, This compound has unique chemical properties. The synthetic route is as follows., Computed Properties of C5H6N2O2

C2-Ocyclopropyl Boc protected amine macrocycle Am (75 mg, 0.093 mmol) is charged in a vial, then a 4 M solution of HCI in dioxane (1 ml_, 4 mmol) is added. The solution is stirred at RT for 1 .5 h, after which a precipitate forms. The solution is evaporated to dryness. 1 -methyl-1 H-pyrazole-3-carboxylic acid R2b (14.0 mg, 0.1 1 1 mmol) is dissolved in DCM (2 ml_), then TEA (51 .6 muIota_, 0.370 mmol) is added followed by TBTU (35.7 mg, 0.1 1 1 mmol). The solution is stirred for 15 mins, after which it is added to the amine hydrochloride in solution in DCM (1 ml_). The solution is stirred at RT for 16 h. The reaction is not complete so additional 1 -methyl-1 H pyrazole-3-carboxylic Acid R2b (3.5 mg, 0.028 mmol), TEA (13.0 muIota_, 0.092 mmol) followed by TBTU (8.9 mg, 0.028 mmol) are added. The solution is stirred at RT for 5 h, concentrated and then the residual is dissolved in DMSO. The resulting solution is filtered through a Millex filter and purified by prep HPLC (Sunfire column, ammonium formate and MeOH). The pure fractions are combined, concentrated, redissolved in MeCN and water, frozen and lyophilized to provide compound 1028. FIA M.S.(electrospray) : 818.4 (M+H)+ Retention time (min) = 5.5 min1H NMR (400 MHz,DMSO-d6): delta 10.80 (bs, 1 H), 8.93 (s, 1 H), 7.84 (d, 1 H, J = 8.9 Hz), 7.76 (d, 1 H, J = 2.4 Hz), 6.74-7.70 (m, 1 Hz), 7.10 (d, 1 H, J = 9.2 Hz), 6.59 (d, 1 H, J = 2.1 Hz), 6.38 (s, 1 H), 5.68-5.54 (m, 1 H), 5.47-5.40 (m, 1 H), 5.10-5.00 (m, 1 H), 4.68-4.56 (m 1 H), 4.50 (qn, 1 H, J = 3.2 Hz) 4.47-4.38 (m, 2H), 4.08-3.96 (m, 1 H), 3.89 (s, 3H), 3.88 (s, 3H), 2.66-2.58 (m, 1 H), 2.47 (s, 3H), 2.40-2.28 (m, 2H), 2.01 -1 .74 (m, 2H), 1 .64-1 .49 (m, 3H), 1 .48-1 .13 (m, 12H), 0.93-0.79 (m, 4H), 0.76- 0.69 (m, 2H).

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 25016-20-0.

Electric Literature of 5334-39-4,Some common heterocyclic compound, 5334-39-4, name is 3-Methyl-4-nitro-1H-pyrazole, molecular formula is C4H5N3O2, 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 tert-butyl 4-(3-methyl-4-nitro-lH- pyrazol-1- yl)piperidine-l- carboxylate and tert-butyl 4-(5-methyl-4-nitro-lH- pyrazol- 1 -yl)piperidine- 1- carboxylate (4.8 g, 15.5 mmol, form step 1) in MeOH (20 mL) was added 10% Pd/C (480 mg), and the resulting mixture was stirred at room temperature under hydrogen atmosphere for 4 hours. The LCMS indicated the starting materials were consumed. After filtration, the filtrate was concentrated to give a mixture of tert-butyl 4-(4-amino-3 -methyl- lH-pyrazol-1- yl) piperidine- 1 -carboxylate and tert-butyl 4-(4-amino-5 -methyl- IH-pyrazol-l-yl) piperidine- 1-carboxylate (4.1 g, Yield: 94%, isomeric ratio: around 5/3 based on HNMR) as light yellow oil. ESI-LCMS (m/z): 281.2 [M+1]

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3-Methyl-4-nitro-1H-pyrazole, its application will become more common.

These common heterocyclic compound, 175137-46-9, name is 5-Cyclopropyl-1H-pyrazol-3-amine, 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. Recommanded Product: 5-Cyclopropyl-1H-pyrazol-3-amine

A mixture of 2,4,6-trichloropyrimidine (30 g, 163 mmol), 5-cyclopropyl-1H-pyrazol-3-ylamine (20 g, 163 mmol), diisopropylethylamine (50 mL, 300 mmol) and 1-butanol (100 mL) was heated to 80 C. for 2 h. The solvents were removed on a rotary evaporator and the residue was taken up in ethyl acetate. The organic solution was washed with water and brine and dried over magnesium sulfate. The residue was concentrated on a rotary evaporator to give the desired product (40.7 g, 92%) as a light yellow solid.

The synthetic route of 5-Cyclopropyl-1H-pyrazol-3-amine 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. 871239-17-7, name is 3-Bromo-1-(2-chlorophenyl)-1H-pyrazole-5-carboxylic acid belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below. Computed Properties of C10H6BrClN2O2

EXAMPLE 3; Preparation of 3-bromo-1- (2-chlorophenyl)-N-[2,4-dichloro carbonyl]phenyl]-1H-pyrazol-5-carboxamide; Step A: Preparation of 2-[3-bromo-1-(2-chlorophenyl)-1H-pyrazol-5-yl]-6,8-dichloro- 4H-3, 1 -benzoxazin-4-one; To a mixture of 3-bromo-1-(2-chlorophenyl)-lH-pyrazole-5-carboxylic acid (i. e. the carboxylic acid product of Example 1, Step E) (3.0 g, 9.44 mmol) and 3,5-dichloroanthranilic acid (1.94 g, 9.44 mmol) in acetonitrile (60 mL) was added 3-picoline (4.81 mL, 49.1 mmol) at room temperature, and the reaction mixture was stirred for 5 minutes. The reaction mixture was cooled to -10 C and methanesulfonyl chloride (1.91 mL, 24.56 mmol) in acetonitrile (5 mL) was added dropwise. The reaction mixture was warmed to room temperature and stirred overnight. The resulting solids were isolated by filtration, washed with water, then dissolved in excess methylene chloride and dried (MgS04). The solvent was evaporated under reduced pressure, and the residual solid was purified by chromatography on silica gel to afford the title compound (2.0 g). 1H NMR (CDC13) No. 8.0 (s, 1H), 7.72 (s, 1H), 7.4-7.55 (m, 4H), 7.28 (s, 1H)

The synthetic route of 871239-17-7 has been constantly updated, and we look forward to future research findings.