反应详情

2.31 g of 8-fluoro-4,5-dihydro-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one was stirred at 95° for 1.5 hours with 8.88 g (35 mmol) of iodine in 25 ml of N,N-dimethylformamide. The reaction mixture was then poured into 300 ml of water, decolorized with sodium thiosulphate solution and extracted four times with methylene chloride. The organic extracts were washed three times with water, dried over magnesium sulphate and evaporated. After recrystallization of the residue from ethyl acetate there was obtained 8-fluoro-4,5-dihydro-3-iodo-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one of melting point 187°-188°.

1. extractionextracted four times with methylene chloride
2. washThe organic extracts were washed three times with water
3. dry with materialdried over magnesium sulphate
4. customevaporated
5. customAfter recrystallization of the residue from ethyl acetate