New downstream synthetic route of 65515-28-8

Statistics shows that 65515-28-8 is playing an increasingly important role. we look forward to future research findings about Methyl 2,6-dichloronicotinate.

Synthetic Route of 65515-28-8, With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.65515-28-8, name is Methyl 2,6-dichloronicotinate, molecular formula is C7H5Cl2NO2, molecular weight is 206.03, as common compound, the synthetic route is as follows.

A 250 mL eggplant flask was sequentially charged with methyl 2,6-dichloronicotinate (2.06 g, 10 mmol), 4-(tertbutyl)phenol (1.50 g, 10mmol), and 12 mL of N, N-dimethylformamide for dissolving them. Triethylamine (1.80 mL, 13mmol) was added dropwise under stirring at room temperature, and after completion of the dropwise addition, triethylenediamine (168 mg, 1.50 mmol) was added. The mixture was stirred at room temperature for 4-5 hours and the solutionchanged from clear to turbid. Thin layer chromatography [V (petroleum ether) / V (ethyl acetate) = 6/1] detected thatmost of the raw material disappeared. Then, 1.30 mL of HOAc, 25 mL of isopropanol and 15 mL of ice water weresequentially added while the solution changed from turbid to clear, and stirred at room temperature for 0.5 hour. 40 mLof water was slowly dropwise added, and after completion of the dropwise addition, stirred at room temperature for 2hours. A large number of white solid precipitated and was filtered. The filter cake was washed with a mixed solution ofisopropyl alcohol / water = 1: 1 and dried under vacuum at 50 C for 8 hours to obtain 2.60 g of methyl 6-(4-(tertbutyl)phenoxy)-2-chloronicotinate as a solid, 81.50%

Statistics shows that 65515-28-8 is playing an increasingly important role. we look forward to future research findings about Methyl 2,6-dichloronicotinate.

Reference:
Patent; Shenyang Sunshine Pharmaceutical Co., Ltd.; ZHOU, Yunlong; CAI, Suixiong; WANG, Guangfeng; JIAO, Lingling; MIN, Ping; JING, Yu; GUO, Ming; (44 pag.)EP3275881; (2018); A1;,
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