Category: 6076-12-6

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. 6076-12-6, name is Ethyl 4-methyl-1H-pyrazole-3-carboxylate, A new synthetic method of this compound is introduced below., Recommanded Product: Ethyl 4-methyl-1H-pyrazole-3-carboxylate

General procedure: A mixture of 1H-imidazole-2-carbaldehyde 40 (200 mg, 2.08 mmol), potassium carbonate (0.8630 g, 6.24 mmol) and 3-(bromomethyl)-1,1′-biphenyl 38 (0.7716 g, 3.12 mmol) in acetonitrile (10 mL) was stirred overnight at room temperature, then the solvent was removed, diluted with water, and extracted with ethyl acetate (3 x 30 mL). The combined organic phases were washed with brine, dried with Na2SO4, filtered, concentrated and purified by silica gel chromatography to afford 44 as a pale yellow solid (527 mg, 97%).

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.

Reference:
Article; Yao, Yiwu; Liao, Chenzhong; Li, Zheng; Wang, Zhen; Sun, Qiao; Liu, Chunping; Yang, Yang; Tu, Zhengchao; Jiang, Sheng; European Journal of Medicinal Chemistry; vol. 86; (2014); p. 639 – 652;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

These common heterocyclic compound, 6076-12-6, name is Ethyl 4-methyl-1H-pyrazole-3-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. 6076-12-6

Ethyl 4-methyl-1 H-pyrazole-3-carboxylate (Intermediate 33) (1.0 g, 6.49 mmol) was dissolved in DMF : H20 (9.0 mL : 1.0 mL) and K20O3(3.58 g, 25.9 mmol) and sodium 2-chloro-2,2-difluoroacetate (Intermediate 35) (3.94 g, 25.9 mmol) were added at 0 C and then the mixture was heated at 130 C for 20 min. The reaction mixture was cooled to RT and ice-cold water was added. The aqueous layer was extracted with EtOAc (3 x 50 mL) and the combined organic layer was washed with brine solution, dried over Na2S04, filtered and concentrated. The residue was purified by column chromatography (Normal-Phase 60-120 mesh silica gel, 25 % EtOAc in hexanes) to give ethyl 1- (difluoromethyl)-4-methyl-1 /-/-pyrazole-3-carboxylate (325 mg, 25 %) as a solid.LCMS (System 3, Method D): m/z 205 (M+H)+(ESI +ve), at 3.77 min, 202 nm.

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 6076-12-6.

6076-12-6, 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. 6076-12-6, name is Ethyl 4-methyl-1H-pyrazole-3-carboxylate, A new synthetic method of this compound is introduced below.

Compound 258.1. Ethyl 5-iodo-4-methyl-lH-pyrazole-3-carboxylate. Into a 250- mL round-bottom flask, was placed a solution of ethyl 4-methyl-lH-pyrazole-3-carboxylate (600 mg, 3.89 mmol) in N,N-dimethylformamide (20 mL). MS (2.2 g, 9.78 mmol) was added and the resulting mixture was stirred for 6 h at 50 C, then quenched with water (10 mL). The mixture was extracted with ethyl acetate (3 x 40 mL) and the combined organic extracts were washed with aqueous a2S203 (sat., 2 x 30 mL) and brine (2 x 20 mL), dried ( a2S04), filtered and concentrated under reduced pressure. The residue was purified by a silica gel chromatography with ethyl acetate/petroleum ether (1 : 10) as eluent to obtain the title compound as a white solid (800 mg, 73%).

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.