反应详情

温度

0 °C

A suspension of 2,3,9,10a-tetrahydrobenzo[b]cyclopenta[e][1,4]diazepin-10(1H)-one (25.00 g, 0.125 mol.) in N,N-dimethylformamide (150 mL) was cooled to 0° C., to which was added sodium hydride (60% liquid paraffin dispersion, 5.00 g, 0.125 mol.). This mixture was stirred for 10 minutes at the same temperature and for 5 minutes at 20° C. This solution was cooled to 0° C., to which was added 4-nitrobenzyl bromide (28.32 g, 0.131 mol.), and the mixture was stirred for 10 minutes at 20° C. The reaction mixture was poured into a saturated aqueous solution of ammonium chloride (500 mL). Resulting precipitate was subjected to filtration, and washed with water, followed by recrystallization from dichloromethane-ethanol to give 29.76 g (yield 71%) of the titled compound. The sample for analylical experiment was prepared by recrystallization of the compound from chloroform-ethanol, m.p. 185°-188° C.

1. temperatureThis solution was cooled to 0° C., to which
2. stirringthe mixture was stirred for 10 minutes at 20° C
3. customResulting precipitate
4. filtrationwas subjected to filtration
5. washwashed with water
6. customfollowed by recrystallization from dichloromethane-ethanol