反应详情

A suspension of 1.1 g (3 mmol) of (S)-1-[(8-chloro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepin-1-yl)carbonyl]imidazole in 10 ml of dry dimethylformamide is treated while stirring with 0.34 g (3 mmol) of potassium t-butylate, the mixture is stirred at room temperature for a further 30 minutes, then poured into 200 ml of water and extracted three times with chloroform. The chloroform solution is washed three times with water, dried over magnesium sulphate and evaporated. After crystallization from ethyl acetate, there is obtained t-butyl 8-chloro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylate of melting point 223°-225°.

1. additionis treated
2. extractionextracted three times with chloroform
3. washThe chloroform solution is washed three times with water
4. dry with materialdried over magnesium sulphate
5. customevaporated
6. customAfter crystallization from ethyl acetate