反应详情

70 g (242 mmol) of 6-iodoisatoic acid anhydride and 24.46 g (242 mmol) of L-azetidine-2-carboxylic acid in 140 ml of dimethyl sulphoxide are stirred at 105° for 2 hours, the dimethyl sulphoxide is removed in vacuo and the residue is heated to 140° in a high vacuum for 2.5 hours. By chromatography on silica gel while eluting with ethyl acetate and subsequent recrystallization from ethyl acetate there is obtained (S)-1,10a-dihydro-5-iodo-azeto[2,1-c][1,4]benzodiazepine-4,10(2H,9H)-dione of melting point 186°-187°.

1. customthe dimethyl sulphoxide is removed in vacuo
2. temperaturethe residue is heated to 140° in a high vacuum for 2.5 hours
3. washBy chromatography on silica gel while eluting with ethyl acetate and subsequent recrystallization from ethyl acetate