反应详情

500 mg of 8-methoxy-1-phenyl-4,5-dihydro-3H-2,3-benzodiazepine-4-thione is stirred in 1.5 ml of ethylene glycol monomethyl ether (Cellosolve® and 548 mg of 2-aminomethyl-2-methyl-1,3-dioxolane while argon is passing through it for 10 hours at 60° C. After filtration and washing with cold ethanol and diisopropyl ether, 550 mg of imino compound, which is dissolved in 10 ml of ethanol, mixed with 10 ml of concentrated hydrocholoric acid and refluxed for 3 hours, is obtained. It is added to water, set at pH 11 and extracted with ethyl acetate. The ethyl acetate phase is washed with water, dried, filtered and concentrated by evaporation. After recrystallization from ethyl acetate/diisopropyl ether, 240 mg of 8-methoxy-3-methy-6-phenyl-11H-imidazo[1,2-c][2,3]benzodiazepine with a melting point of 140° C. is obtained.

1. filtrationAfter filtration
2. washwashing with cold ethanol and diisopropyl ether, 550 mg of imino compound, which
3. dissolutionis dissolved in 10 ml of ethanol
4. additionmixed with 10 ml of concentrated hydrocholoric acid
5. temperaturerefluxed for 3 hours
6. customis obtained
7. extractionextracted with ethyl acetate
8. washThe ethyl acetate phase is washed with water
9. customdried
10. filtrationfiltered
11. concentrationconcentrated by evaporation
12. customAfter recrystallization from ethyl acetate/diisopropyl ether, 240 mg of 8-methoxy-3-methy-6-phenyl-11H-imidazo[1,2-c][2,3]benzodiazepine with a melting point of 140° C.
13. customis obtained