A preparation method of 4,5-dihydro-1h,3h-pyrrolo[1,2-a][1,4]diazepine-2,4-dicarboxylate-2-tert-butyl ester
A technology of diazepine and tert-butyl ester, which is applied in the field of preparation of dihydropyrrolodiazepine dicarboxylate-2-tert-butyl ester, can solve the problems of no suitable industrial synthesis method, and achieve a synthetic route Short, easy-to-response, and easy-to-operate effects
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[0010] Example 1: a. Dissolve compound 1 (100.00 g, 1.05 mol) in acetonitrile (500 mL), add potassium carbonate (218.00 g, 1.58 mol) and stir for half an hour, then slowly add compound 2 dropwise at 0°C, after the dropwise addition is completed The reaction was stirred at 20°C for 12 hours. TLC (petroleum ether / ethyl acetate volume ratio=2 / 1) showed that the reaction was complete. Water was added to the reaction system, and then extracted three times with ethyl acetate. The combined organic phases were purified by silica gel column chromatography to obtain compound 3 (186.83 g, 901.56 mmol), with a yield of 85.86%.
[0011] b. Dissolve compound 3 (186.83 g, 901.56 mmol) and benzylamine (106.26 g, 991.71 mmol) in ethanol (500 mL), react at 20°C for half an hour, then add sodium borohydride (20.46 g, 540.94 mmol) at 20 °C stirring was continued for 30 minutes. TLC (petroleum ether / ethyl acetate volume ratio=5 / 1) showed that the starting material was consumed completely. The r...
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