反应详情

To a suspension of 5.0 g (15.5 mmol) of the known 1-(4-nitrophenyl-4-methyl-7,8-methylenedioxy-5H-2,3-benzodiazepine (French patent specification No. 85,09793) in 380 ml of ethanol first 22.5 ml (0.278 mol) of concentrated hydrochloric acid were added at constant stirring whereupon a solution was formed within a few minutes, then 11.5 g (0.3 mole) of sodium borohydride were charged into the solution portionwise during 30 minutes. Stirring was continued for 15 minutes, then the orange-coloured precipitate formed was filtered and extracted on the filter with 4×30 ml of chloroform. The combined chloroform filtrate was evaporated under reduced pressure, the crystalline residue was brought to a filter with 200 ml of distilled water, then washed with 3×20 ml of distilled Water and dried at 80°-100° C. to yield 4.90 g (97.2%) of the aimed product, m.p.: 162°-164° C.

1. additionTo a suspension of 5.0 g (15.5 mmol) of the
2. additionwere added
3. customwas formed within a few minutes
4. stirringStirring
5. customthe orange-coloured precipitate formed
6. filtrationwas filtered
7. extractionextracted on the
8. filtrationfilter with 4×30 ml of chloroform
9. customThe combined chloroform filtrate was evaporated under reduced pressure
10. filtrationa filter with 200 ml of distilled water
11. washwashed with 3×20 ml of distilled Water
12. customdried at 80°-100° C.