反应详情

A mixture of 2.69 g (15 mmole) of N-formyl-N-phenyl-glycine prepared in Reference Example 3, 5.47 g (55.8 mmole) of ethyl propiolate, and 15 ml of acetic anhydride was stirred using a magnetic stirrer over an oil bath at 130° C. for 22 hours. The reaction mixture was concentrated under vacuum. 22 ml of toluene was added to the residue and the mixture was evaporated under reduced pressure. This procedure was repeated to obtain a brown oily substance. This oily substance was purified using silica gel column chromatography (No. 9385 silica gel, manufactured by Merck Co., eluted with ethyl acetate:hexane=1:5 v/v) to obtain 2.8949 (yield 89.6%) of a light-yellow oil of the title compound.

1. customat 130° C.
2. customfor 22 hours
3. concentrationThe reaction mixture was concentrated under vacuum
4. addition22 ml of toluene was added to the residue
5. customthe mixture was evaporated under reduced pressure
6. customto obtain a brown oily substance
7. customThis oily substance was purified
8. wash, eluted with ethyl acetate