反应详情

To 100 ml of dimethylformamide, there were added 7.45 g of N-cyclohexyl-N-(2-hydroxyethyl)-4-(6-carbostyriloxy)butyramide and 0.5 ml of triethylamine, then the whole mixture was heated at 80° to 90° C. on an oil bath. Next, 1.8 g of diketene were added dropwise to the reaction mixture, then the mixture was stirred for 1 hour at the same temperature. The reaction mixture was concentrated then was purified by a silica gel column chromatography (eluant: chloroform/methanol=50/1), and the solvent was removed by distillation under reduced pressure to yield 6.33 g of N-(2-acetoacetoxyethyl)N-cyclohexyl-4-(6-carbostyriloxy)butyramide in the form of a brownish oily substance.

1. temperaturethe whole mixture was heated at 80° to 90° C. on an oil bath
2. concentrationThe reaction mixture was concentrated
3. customthen was purified by a silica gel column chromatography (eluant: chloroform/methanol=50/1)
4. customthe solvent was removed by distillation under reduced pressure