反应详情

温度

100 °C

4.46 g (10 mmoles) of (±)-3-acetyl-7-bromo4,5-dihydro-1-(3-methyl-4-nitrophenyl)-4-methyl-8-methoxy-3H-2,3-benzo-diazepine are dissolved in 190 cm3 of methyl cellosolve, then 2.1 g (15 mmoles) of potassium carbonate and 1.8 g of 10% palladium/charcoal catalyst and, under vigorous stirring, 1.95 cm3 (40 mmoles) of 98% hydrazine hydrate are added. The reaction mixture is stirred at 100° C. for 1 hour, the catalyst is filtered, the filtrate is evaporated, and the residue is rubbed with 50 cm3 of water to obtain solid matter. The crude product is purified by chromatography over a column containing silica gel and using a mixture of ethyl acetate and hexane, then the product is recrystallized from acetonitrile. Thus, 1.6 g (47%) of the title compound are obtained in the form of cream coloured solids melting at 169–171° C.

1. filtrationthe catalyst is filtered
2. customthe filtrate is evaporated
3. customto obtain solid matter
4. customThe crude product is purified by chromatography over a column
5. additioncontaining silica gel
6. additiona mixture of ethyl acetate and hexane
7. customthe product is recrystallized from acetonitrile