反应详情

A mixture of 15 g. (0.05 mol) of 1,3-dihydro-1-methyl-7-nitro-5-phenyl-2H-1,4-benzodiazepin-2-one, 250 ml. of tetrahydrofuran, 250 ml. of methanol, 56 g. of stannous chloride dihydrate and 68 g. of sodium acetate trihydrate was stirred under nitrogen for 3 hours. 1 l. of methylene chloride and 15 ml. of concentrated ammonia was added. The inorganic material was separated by filtration over celite. The filtrate was washed with 1N sodium hydroxide solution, was dried over sodium sulfate and evaporated. Crystallization of the residue from methylene chloride and recrystallization from ethanol/methylene chloride yielded light yellow product with m.p. 211°-213°.

1. additionA mixture of 15 g
2. customThe inorganic material was separated by filtration over celite
3. washThe filtrate was washed with 1N sodium hydroxide solution
4. dry with materialwas dried over sodium sulfate
5. customevaporated
6. customCrystallization of the residue
7. customfrom methylene chloride and recrystallization from ethanol/methylene chloride
8. customyielded light yellow product with m.p. 211°-213°