反应详情

温度

0 °C

1 g of (S)-5-(o-fluorophenyl)-1,3-dihydro-1,3-dimethyl-7-nitro-2H-1,4-benzodiazepin-2-one is introduced portionwise into 10 ml of concentrated hydrochloric acid while cooling with ice at 0° C. The solution obtained is treated slowly at 0° C. with 2 g of stannous chloride, stirred for 30 minutes while cooling with ice, poured into ice/sodium bicarbonate solution and extracted several times with methylene chloride. The organic phase is dried over sodium sulphate, filtered and concentrated. After crystallisation from ether, there is obtained (S)-7-amino-5-(o-fluorophenyl)-1,3-dihydro-1,3-dimethyl-2H-1,4-benzodiazepin-2-one which crystallises with 1 mol of ether; melting point 100°-110° C. (with decomposition); [α]25D =+77.1° (in methylene chloride; 1%).

1. customThe solution obtained
2. temperaturewhile cooling with ice
3. extractionextracted several times with methylene chloride
4. dry with materialThe organic phase is dried over sodium sulphate
5. filtrationfiltered
6. concentrationconcentrated
7. customAfter crystallisation from ether