反应详情

A solution of 1,1-dimethylethyl-7-{(3E)-3-[{[(1,1 dimethylethyl)oxy]carbonyl}(methyl)hydrazono]butanoyl}-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate (0.5 g) (intermediate 2) in dichloromethane (5 ml) was added dropwise to trifluoroacetic acid (10 ml) under vigorous stirring. After 1 h the reaction mixture was concentrated in vacuo and sodium hydroxide (1N) was added until pH ˜12, then the mixture was extracted twice with dichloromethane. The organic phase was dried with sodium sulphate and evaporated to give the title compound (0.26 g).

1. concentrationAfter 1 h the reaction mixture was concentrated in vacuo and sodium hydroxide (1N)
2. additionwas added until pH ˜12
3. extractionthe mixture was extracted twice with dichloromethane
4. dry with materialThe organic phase was dried with sodium sulphate
5. customevaporated