反应详情

To a solution of 0.56 g 4-hydroxy-5-[(4-methoxy-7-morpholin-4-yl-benzothiazole-2-carbonyl)-amino]-azepane-1-carboxylic acid tert-butyl ester in 10 ml dimethylsulfoxide were added 0.93 ml triethylamine, 10 ml dichlotomethane and a solution of 0.58 g sulfur trioxide pyridine complex in 8 ml dimethylsulfoxide. The mixture was stirred for 18 hours at room temperature. Extraction with water/ ethylacetate and chromatography on silicagel with dichloromethane/methanol 97:3 yielded 0.49 g (87%) 4-[(4-methoxy-7-morpholin-4-yl-benzothiazole-2-carbonyl)-amino]-5-oxo-azepane-1-carboxylic acid tert-butyl ester as yellow solid; M.p.: 95–97° C.; MS (ISP): m/e=505 (M+H+).

1. extractionExtraction with water/ ethylacetate and chromatography on silicagel with dichloromethane/methanol 97:3