反应详情

A solution of 2 g. of ethyl 2'-benzoyl-4'-chloro-mesoxalanilate-2-oxime in 40 ml. of methylene chloride is treated with 2 g. of zinc dust. 4 ml. of glacial acetic acid are added dropwise within 5 minutes with stirring. After the addition, the mixture is stirred at room temperature for 1 hour. The reaction mixture is filtered and the filtrate evaporated. The residue is boiled under reflux for 2 hours in 20 ml. of benzene and 2 ml. of glacial acetic acid. The reaction mixture is washed out with 10% soda solution, dried over sodium sulphate and evaporated. Crystallization of the residue from alcohol yields ethyl 7-chloro-1,3-dihydro-5-phenyl-2H-1,4-benzodiazepin-2-one-3-carboxylate, m.p. 232°-234°. Further material crystallizes from the mother liquor.

1. additionAfter the addition
2. stirringthe mixture is stirred at room temperature for 1 hour
3. filtrationThe reaction mixture is filtered
4. customthe filtrate evaporated
5. temperatureunder reflux for 2 hours in 20 ml
6. washThe reaction mixture is washed out with 10% soda solution
7. dry with materialdried over sodium sulphate
8. customevaporated
9. customCrystallization of the residue from alcohol