Day: February 9, 2021

Reference of 57097-81-1, A common heterocyclic compound, 57097-81-1, name is 3-Bromo-5-methyl-1H-pyrazole, molecular formula is C4H5BrN2, 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 3-bromo-5-methyl-1H-pyrazole (from Ark Pharm, 6.4 g, 40 mmol) in tetrahydrofuran (263 mL) at 0 C. was added sodium hydride (3.2 g, 80 mmol). After stirring for 30 min, [beta-(trimethylsilyl)ethoxy]methyl chloride (8.4 mL, 48 mmol) was added and the reaction mixture was allowed to warm to room temperature over 2 h. The reaction mixture was diluted with ethyl acetate and water. The aqueous layer was extracted with ethyl acetate. The combined organic layers were washed with brine, dried over Na2SO4, filtered and concentrated. The crude was purified with flash chromatography (eluting with a gradient of 0-15% ethyl acetate in hexanes) to give the desired product as colorless oil (12 g, 100%). LCMS calculated for C10H20BrN2OSi (M+H)+: m/z=291.1. Found: 291.0

The synthetic route of 57097-81-1 has been constantly updated, and we look forward to future research findings.

Electric Literature of 176969-34-9, The chemical industry reduces the impact on the environment during synthesis 176969-34-9, name is 3-(Difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid, I believe this compound will play a more active role in future production and life.

To a solution of 600 mg of 3-difluoromethyl-1- methyl-lH-pyrazole-4-carboxylic acid [compound (III)] and a catalytic amount of N, -dimethylformamide in dichloromethane (7 mL) , 450 mg of thionyl chloride were added dropwise. The mixture was refluxed for 2h. The reaction was monitored by GC/MS . The solvent was evaporated in vacuo. The crude acid chloride obtained was used in the following step.

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, 3-(Difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid, other downstream synthetic routes, hurry up and to see.

Adding a certain compound to certain chemical reactions, such as: 313735-62-5, name is 4-Bromo-1-isopropylpyrazole, 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 313735-62-5, SDS of cas: 313735-62-5

To a degassed (N2 bubbling) solution of the compound of Intermediate Example 12(a) 4-bromo-1-isopropyl-1H-pyrazole (1.5 g, 7.9 mmol) in 1,4-dioxane (30 ml) were added 4,4,4′,4′,5,5,5′,5′-octamethyl-2,2′-bi(1,3,2-dioxaborolane) (3 g, 11.84 mmol, 1.5 eq.), Pd(dppf)Cl2 (0.64 g, 0.79 mmol, 0.1 eq.) and potassium acetate (1.93 g, 19.74 mmol, 2.5 eq.) using the procedure of Intermediate Example 1(b). The solvent was distilled off to afford the product in 67% yield (1.2 g). LC-MS (ESI): Calculated mass: 236.12; Observed mass: 237.1 [M+H]+ (rt: 1.41 min).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Bromo-1-isopropylpyrazole, and friends who are interested can also refer to it.

Application of 20583-33-9, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 20583-33-9 name is 1-(1H-Pyrazol-3-yl)ethanone, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

Reference Synthesis Example 118 (0768) 3-(1,1-Difluoroethyl)-1H-pyrazole (0769) To a dichloroethane solution (6.0 mL) of 1-(1H-pyrazol-3-yl)ethanone (300 mg, 2.73 mmol) and bis(2-methoxyethyl))amino-sulfur trifluoride (1.11 mL, 5.99 mmol), one drop of ethanol was added at 0 C. and the resultant mixture was stirred at room temperature for 1 hour and 30 minutes. After completion of the reaction, the reaction solution was added dropwise to saturated sodium bicarbonate aqueous solution at 0 C. After adding dichloromethane, the resultant mixture was washed with saturated sodium chloride aqueous solution. The organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure. The obtained residue was purified by column chromatography (hexane/ethyl acetate=3/1) to obtain the title compound (145 mg, yield 41%).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-(1H-Pyrazol-3-yl)ethanone, and friends who are interested can also refer to it.

Adding a certain compound to certain chemical reactions, such as: 36650-74-5, name is 1H-Pyrazole-3-carbonitrile, 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 36650-74-5, Product Details of 36650-74-5

General procedure: A mixture of cyanopyrazole 8 or 11 (0.05 mol), NaN3 (4.23 g, 0.065 mol), triethylamine hydrochloride (8.94 g, 0.065 mol), and toluene (150 ml) was refluxed for 10 h in the case of compound 9 or 8 h in the case of compound 12. The reaction mixture was cooled, stirred, and diluted with 2 (200-500 ml) until complete dissolution of the precipitate. The aqueous layer was separated and acidified with HCl to 1-2. The precipitate that formed was filtered off, washed with cold water, and air-dried. In the case of compound 12, the filtrate was additionally extracted with EtOAc (350 ml), and the organic layer was dried over anhydrous Na2SO4. The solvent was removed under vacuum, providing a second crop of the product. Both precipitates were combined and air-dried. 5-(1-Pyrazol-3(5)-yl)tetrazole (9). Yield 5.37 g (79%), decomp. temp. 272-274C (EtOH). IR spectrum, nu, cm-1: 3379 (s), 3222 (s), 3125 (s), 2975 (m), 2870 (m), 2757 (m), 2637 (s), 2520 (m), 1871 (vs), 1614 (s), 1456 (s), 1347 (w), 1223 (m), 1196 (m), 1068 (s), 1034 (s), 942 (m), 922 (m), 782 (s), 750 (s), 709 (m), 608 (m). Mass spectrum, m/z: 136 [M]+. Found, %: C 35.24; H 2.96; N 61.42. 4H4N6. Calculated, %: C 35.30; H 2.96; N 61.74.

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.

Related Products of 1280210-79-8, These common heterocyclic compound, 1280210-79-8, name is tert-Butyl 4,6-dihydropyrrolo[3,4-c]pyrazole-5(2H)-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.

To a solution of tert-butyl 4,6-dihydropyrrolo[3,4- c]pyrazole-5(2H)-carboxylate (250 mg, 1.2 mmol) in DMF (5 mL) was added NaH (96 mg, 2.4 mmol (60% in mineral oil)), with the reaction mixture being cooled with an ice bath. The resulting mixture was stirred at room temperature for 1 h, whereupon iodoethane (374 mg, 2.4 mmol) was added, and the resulting reaction mixture was stirred at room temperature for 2 h. The reaction mixture was then diluted with water (10 mL) and extracted with EtOAc (10 mL x 3). The combined organic layers were washed with brine (10 mL x 3), dried over anhydrous Na2S04 and then concentrated in vacuo to give 135 and 135-A as a crude product. MS 238.2 [M + H]+. (0141) [0090] Synthesis of 136 and 136- A. To a solution of 135 and 135-A (1.2 mmol, crude product from last step) in DCM (6 mL) was added TFA (2 mL) dropwise while the reaction mixture was cooled with an ice bath. The reaction mixture was stirred at room temperature 1 h, whereupon the solvent was removed in vacuo to give 136 and 136-A as a crude product which was used in the next step without further purification. MS 138.2 [M + H]+. (0142) [0091] Synthesis of 137. A mixture of 136 and 136-A (1.2 mmol, crude product from last step) and A3 (491 mg, 1.0 mmol) in DMSO (10 mL) was stirred at room temperature for 10 min, then Na2C03 (848 mg, 8.0 mol) was added, and the reaction mixture was stirred at room temperature for 2 h. The reaction mixture was then diluted with water (20 mL) and extracted with EtOAc (20 mL x 3). The combined organic layers were washed with brine (20 mL x 3), dried over anhydrous Na2S04 and then concentrated in vacuo. The crude residue was purified by column chromatography on silica gel (DCM : MeOH = 100 : 1 ~ 50 : 1) to give a crude product which was a mixture of the regioisomers 137 and 137-A. The crude product was further purified by Prep-TLC (DCM : MeOH = 30 : 1) to give 137 (150 mg, 36%) as a yellow solid. MS 415.1 [M + H]+.

The synthetic route of 1280210-79-8 has been constantly updated, and we look forward to future research findings.

Adding a certain compound to certain chemical reactions, such as: 31108-57-3, name is 1H-Pyrazole-4-carbonitrile, 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 31108-57-3, Computed Properties of C4H3N3

Preparation 8 ethyl 2-(4-cyano-lH-pyrazol-l-yl)acetate [0151] Combined lH-pyrazole-4-carbonitrile (0.432 g, 4.64 mmol) in acetone (9.28 mL), potassium carbonate (1.924 g, 13.92 mmol) and ethyl 2-bromoacetate (1.027 mL, 9.28 mmol). The reaction mixture was stirred at room temperature overnight, then concentrated in vacuo, diluted with EtOAc (10 mL), washed with water (10 mL), dried (MgS04) and concentrated in vacuo to give a residue. The residue was purified using flash column chromatography on silica gel (EtOAc in heptane, 10-50% gradient) to give a white solid. The solid was suspended in heptane and then filtered and dried to give the title compound (0.4314 g, 51.9 % yield) as a white solid. XH NMR (400 MHz, DMSO-i) delta ppm 1.21 (t, J=7.20 Hz, 3 H) 4.17 (q, J=7.07 Hz, 2 H) 5.19 (s, 2 H) 8.11 (s, 1 H) 8.57 (s, 1 H). MS m/z [M+H]+ 180.

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.

Related Products of 132712-71-1, These common heterocyclic compound, 132712-71-1, name is 3-Methyl-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.

General procedure: Dichloromethane (10 mL) was taken in a round-bottomed flask,into which 1.0 equivalent (1 mmol) of triethylamine and pyrazolonewere poured. The mixture was stirred for 2 min without heating. To this mixture, 1.0 equivalent of corresponding presynthesized benzylidene from malononitrile was added. Then the mixture was agitated for 25-30 min. The reaction was observed by TLC. The desired products appeared as precipitates. The precipitates were washed with water to remove the unreacted pyrazolone to obtain pure products. Melting points were recordedfor crystalline substances.

Statistics shows that 3-Methyl-1H-pyrazol-5-ol is playing an increasingly important role. we look forward to future research findings about 132712-71-1.

Electric Literature of 175137-46-9,Some common heterocyclic compound, 175137-46-9, name is 5-Cyclopropyl-1H-pyrazol-3-amine, molecular formula is C6H9N3, 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 flask was added Pd(OAc)2 (22.4 mg, 0.1 mmol), (biphenyl-2- ylmethylene)bis(dimethylphosphine) (60 mg, 0.2 mmol) and sodium tert-butoxide (240 mg, 2.5 mmol). The flask was sealed and refilled with N2. To the mixture was added a solution of EPO 6-bromo-N-(4-fluorobenzyl)pyridin-2-amine (Method 19; 281 mg, 1.0 mmol) and 5- cyclopropyl-lH-pyrazol-3 -amine (123 mg, 1.0 mmol) in toluene (5 ml). The reaction mixture was heated at 110C overnight. The solvent was removed and EtOAc was added and the mixture was washed with brine and was concentrated. Semi-prep HPLC (Gilson) purification gave the title compound (6.4 mg, 2%). 1H NMR (CDCl3) delta 0.65 (m, 2H), 0.95 (m, 2H), 1.80 (m, IH), 4.43 (m, 2H), 4.91 (br s, IH), 5.60 (br s, IH), 5.80 (m, IH), 6.18 (m, IH), 6.73 (m, IH), 7.00 (m, 2H), 7.25 (m, 3H).

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

Adding a certain compound to certain chemical reactions, such as: 1314987-79-5, name is tert-Butyl 3-(4-nitro-1H-pyrazol-1-yl)azetidine-1-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 1314987-79-5, COA of Formula: C11H16N4O4

B) tert-butyl 3-(4-amino-1H-pyrazol-1-yl)azetidine-1-carboxylate To a solution of tert-butyl 3-(4-nitro-1H-pyrazol-1-yl)azetidine-1-carboxylate (5.3 g) obtained in Step B of Example 131 in ethanol (30 mL) was added 5% palladium-carbon (4.2 g), and the mixture was stirred at room temperature for 2 hr under hydrogen atmosphere (at normal pressures). The palladium-carbon was removed by filtration through Celite, the solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (NH, hexane/ethyl acetate) to give the title compound (2.1 g). 1H NMR(300 MHz, DMSO-d6)delta1.39 (9H, s), 3.89 (2H, s), 3.98-4.08 (2H, m), 4.14-4.26 (2H, m), 4.92-5.06 (1H, m), 7.03 (1H, s), 7.13 (1H, d, J = 0.8 Hz).

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-(4-nitro-1H-pyrazol-1-yl)azetidine-1-carboxylate, other downstream synthetic routes, hurry up and to see.