反应详情

A solution of 6-phthalimidohexanoyl chloride (2 g.) in dry toluene was added to an ethereal solution of diazoethane at -78° C. and the mixture was allowed to warm to room temperature and stand for 15 hours. On standing a solid crystallized out of solution. The reaction mixture was filtered and the filtrate evaporated to dryness giving 1.43 g. of yellow-green oil. This oil was then dissolved in acetone and concentrated hydrochloric acid added until effervescence ceased. The resulting yellow-brown solution was then evaporated to dryness and azeotroped three times with toluene to give N-(7-chloro-6-oxooctyl)phthalimide (1.4 g.) which was used without further purification.

1. customcrystallized out of solution
2. filtrationThe reaction mixture was filtered
3. customthe filtrate evaporated to dryness
4. customgiving 1.43 g
5. customThe resulting yellow-brown solution was then evaporated to dryness
6. customazeotroped three times with toluene