Day: December 14, 2020

118430-74-3, 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. 118430-74-3 name is 3-Cyclopropyl-1-methyl-1H-pyrazol-5-amine, 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.

A mixture of ferf-butyl 2-(2-(5-bromo-3′-(((tert-butoxycarbonyl)amino)methyl)-5′-fluoro- [1 ,1 ‘-biphenyl]-3-ylcarboxamido)phenyl)acetate (Example 11-B) (100 mg, 0.163 mmol), 3- cyclopropyl-1 -methyl-1 H-pyrazol-5-amine (CAS 118430-74-3) (44.7 mg, 0.326 mmol), Cs2C03 (159 mg, 0.489 mmol) and BrettPhos palladacycle (CAS 1 148148-01-9) (6.51 mg, 8.15 pmol) in CH3CN (2 mL) was heated in a microwave at 160 C for 60 min. The mixture was diluted with EtOAc and water, acidified with 1 N HCI to pH 5. The layers were separated and the aqueous layer was extracted with EtOAc. The combined organic layers were concentrated and the residue was purified by HPLC (Method B) to provide the title compound. MS (ESI+) m/z 670.8 (M+H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-Cyclopropyl-1-methyl-1H-pyrazol-5-amine, and friends who are interested can also refer to it.

The chemical industry reduces the impact on the environment during synthesis 51516-67-7, name is 5-Amino-1-(4-chlorophenyl)-1H-pyrazole-4-carbonitrile, I believe this compound will play a more active role in future production and life. 51516-67-7

General procedure: A mixture of theintermediate compounds 2 (1 mmol) and 3 (1 mmol) in ethanol(10 mL) was stirred at reflux for 2 h. After cooling to roomtemperature, the precipitated solid was filtered, and thenrecrystallized from ethanol to give the title compounds 5a-5p.

The chemical industry reduces the impact on the environment during synthesis 51516-67-7. I believe this compound will play a more active role in future production and life.

Some common heterocyclic compound, 3463-30-7, name is 1-(4-Nitrophenyl)-1H-pyrazole, molecular formula is C9H7N3O2, 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. 3463-30-7

Reference Example 13 4-(Pyrazol-1-yl)phenylamine Under hydrogen atmosphere, an ethanol solution (80 ml) of 1-(4-nitrophenyl)pyrazole (2.91 g) and 5% palladium-carbon (1.4 g) was stirred at room temperature for 24 hours. After filtration of the catalyst, the filtrate was concentrated under reduced pressure and then purified by flash silica gel column chromatography (hexane:ethyl acetate = 1:1) to obtain the title compound (2.45 g) as a colorless oil. 1H-NMR (400 MHz, CDCl3) delta: 3.73 (2H, br s), 6.41 (1H, br s), 6.75 (2H, d, J=8.5 Hz), 7.44 (2H, d, J=8.5 Hz), 7.67 (1H, s), 7.78 (1H, s).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3463-30-7, its application will become more common.

852227-86-2, 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. 852227-86-2 name is 5-(Chloromethyl)-1,3-dimethyl-1H-pyrazole, 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.

A mixture of 3-[(1 -methylpyrazol-4-yl)methyl]-2,4-dioxo-N-[1 – (trideuteriomethyl)cyclopropyl]- 1H -quinazoline-6-sulfonamide (100 mg, 0.25 mmol), 5- (chloromethyl)-1 ,3-dimethyl- 1H -pyrazole (37 mg, 0.25 mmol), potassium carbonate (70 mg, 0.51 mmol) and potassium iodide (42 mg, 0.25 mmol) in DMF (2 mL) was heated with agitation in the microwave at 80 C for 30 minutes. The solvent was removed in vacuo and the residue purified by prep HPLC (high pH) to give the desired product (68 mg, 0.136 mmol, 53%) as a white powder

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 5-(Chloromethyl)-1,3-dimethyl-1H-pyrazole, and friends who are interested can also refer to it.

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. 49633-25-2 name is 3-Isopropylpyrazole, 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. 49633-25-2

Part A – 4-Bromo-3-isopropylpyrazole To a stirred solution of sodium acetate (19.7 g., 0.24 mole) in acetic acid (100 ml.) and water (15 ml.), 3-isopropylpyrazole (11.0 g., 0.1 mole) was added, followed by dropwise addition of bromine (16.0 g., 0.11 mole) keeping the internal temperature below 15 C. The mixture was kept at 25 C. for 15 hours, treated with water (200 ml.) and extracted with ethyl ether (3 * 50 ml.), and the ether layer washed with water (1 * 50 ml.) dried, (sodium sulfate) and evaporated under reduced pressure. The resultant pale yellow oil was distilled to give 4-bromo-3-isopropylpyrazole (15.3 g., 81%) with a boiling point of 85 C. at 0.06 mm Hg. Analysis: Calc’d. for C6 H9 BrN2: C, 38.11; H, 4.80; N, 14.82; Br, 42.27. Found: C, 37.91; H, 4.89; N, 14.83; Br, 42.15.

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

A common heterocyclic compound, 3463-30-7, name is 1-(4-Nitrophenyl)-1H-pyrazole, molecular formula is C9H7N3O2, 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. 3463-30-7.

Compound 11-b (1.0 g, 5.29 mmol) and ammonium chloride (0.7 g, 13.23 mmol) were dissolved in 50percent ethanol-water (20 mL). Zn-powder (0.9 g, 13.23 mmol) was then added. The mixture was refluxed for 30 minutes. After cooled to room temperature, the mixture was filtrated, and the filter cake was washed with ethanol (10 mL). The combined filtrate were concentrated under reduced pressure, and the residue was diluted with water (50 mL) and extracted with ethyl acetate (50 mL¡Á3). The organic layer was dried over anhydrous sodium sulfate. After filtration, the filtrate was concentrated under reduced pressure to give yellow solid 11-a (670 mg, yield: 80percent), which was used directly for the next step without purification. LC-MS (ESI): m/z=160 [M+H]+.

The synthetic route of 1-(4-Nitrophenyl)-1H-pyrazole has been constantly updated, and we look forward to future research findings.

A common compound: 162758-35-2, name is 5-(4-Chlorophenyl)-1-(2,4-dichlorophenyl)-4-methylpyrazole-3-carboxylic acid, belongs to pyrazoles-derivatives compound, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below. 162758-35-2

To a solution of the compound NDS-100226 (76 mg, 0.20 mmol)in dry dichloromethane, was added N-(3-Dimethylaminopropyl)-N’-ethylcarbodiimide hydrochloride (EDC.HC1, 40 mg, 0.26 mmol), Hydroxybenzotriazole (HOBt, 35 mg, 0.26 mmol) and diisopropylethyl amine (0.1 mL, 0.60 mmol) at 0C. Then the amine 3 was added and stirred at RT for 6 h. To the reaction mixture water was added and the organic layer was separated, washed with saturated NaHC03, IN HQ, dried over Na2S04 and concentrated under reduced pressure. This crude mixture was purified by column chromatography to give the title compound NDS-100240 (90 mg) as a white fluffy solid in 89% yield. NMR (400 MHz, CDQ3): delta 7.44 (d, J = 1.8 Hz, 1H), 7.32-7.29 (m, 4H), 7.06 (d, J = 8.3 Hz, 2H), 3.21 (t, J = 6.0 Hz, 411), 2.37 (s, 3H), 0.97 (t, J = 6.3 Hz, 4H), 0.10 (s, 6H) ); 13C NMR (100 MHz, CDC13): 6 159.9, 144.4, 142.9, 135.9 (2C), 134.9, 132.9, 130.8 (2C), 130.5, 130.3, 128.9 (2C), 127.8, 127.2, 1 18.2, 55.4, 13.2, 9.3, -3.5 (2C).

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, 162758-35-2, other downstream synthetic routes, hurry up and to see.

612511-81-6,Some common heterocyclic compound, 612511-81-6, name is (1-Methyl-1H-pyrazol-3-yl)methanamine, molecular formula is C5H9N3, 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 the solution of 4-bromo-6-(((1S,2S)-2-(5-methoxypyridin-2-yl)cyclopropyl) methoxy)-2-methylpyridazin-3(2H)-one (73 mg, 0.2 mmol) in toluene (4 mL) underNz, (1-methyl-1Hpyrazol-3-yl)methanamine (22 mg, 0.2 mmol), Pd2(dba)3 (18 mg, 0.02 mmol), BINAP (18 mg,20 0.03 mmol) and Na01Bu (29 mg, 0.3 mmol) were added. After the reaction mixture was stirred at85 ¡ãC for 4 h, 15 mL water was added. The mixture was extracted with EtOAc (3 x 10 mL). Thecombined organics were dried over MgS04, filtered and concentrated in vacuo. The residue waspurified by Pre-HPLC to afford the title compound as a solid. 1H NMR (400 MHz, MeOD) o8.06 (d, 1H), 7.50(d, 1H), 7.30 (dd, 1H), 7.17 (d, 1H), 6.21 (d, 1H), 5.83 (s, 1H), 4.32 (s, 2H),25 4.18-4.14 (m, 1H), 4.06-4.02 (m, 1H), 3.87 (s, 3H), 3.84 (s, 3H), 3.62 (s, 3H), 2.09 -2.04 (m,1H), 1.76- 1.72(m, 1H), 1.20-1.15 (m, 1H), 1.05-1.00 (m, 1H); LRMS m/z (M+H) 397.2 found,3 97.19 required.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 612511-81-6, its application will become more common.

71229-85-1, The chemical industry reduces the impact on the environment during synthesis 71229-85-1, name is 4-Bromo-1-ethyl-1H-pyrazole, I believe this compound will play a more active role in future production and life.

To a degassed (N2 bubbling) solution of 4-bromo-1-ethyl-1H-pyrazole (2 g, 11.42 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) (4.35 g, 17.14 mmol, 1.5 eq.), Pd(dppf)Cl2 (0.93 g, 1.14 mmol, 0.1 eq.) and potassium acetate (2.79 g, 28.55 mmol, 2.5 eq.) using the procedure of Intermediate Example 1(b). The solvent was distilled off to give the product in 88% yield (2.2 g). LC-MS (ESI): Calculated mass: 222.09; Observed mass: 223.3 [M+H]+ (rt: 0.83 min).

The chemical industry reduces the impact on the environment during synthesis 71229-85-1. I believe this compound will play a more active role in future production and life.

155377-19-8, 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. 155377-19-8, name is Ethyl 3-(trifluoromethyl)pyrazole-4-carboxylate, A new synthetic method of this compound is introduced below.

Example 12 Ethyl 1-(5-iodo-2-isopropylthio-6-trifluororethylpyrimidin-4-yl)-3-trifluoromethyl-1H-pyrazol-4-carboxylate 4-Chloro-5-iodo-2-isopropylthio-6-trifluoromethylpyrimidine (0.30 g) was dissolved in dimethylsulfoxide (3.0 ml) and ethyl 3-trifluoromethyl-1H-pyrazole-4-carboxylate (0.16 g) and 1,8-diazabicyclo-[5,4,0]-under-7-ene (0.12 g) was added at room temperature with stirring. The mixture was heated to 80 C. and stirred for 2 hr. After cooling to room temperature, the mixture was added water and extracted with benzene. The benzene layer was washed with water and brine, respectively and dried over magnesium sulfate. The solvent was removed under reduced pressure. The residue was purified by silica gel column chromatography (hexane-ethyl acetate) to give ethyl 1-(5-iodo-2-isopropylthio-6-trifluoromethylpyrimidin-4-yl)-3-trifluoromethyl-1H-pyrazole-4-carboxylate (0.30 g) as colorless crystalline solid, mp 107-108 C.

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.