反应详情

温度

28 °C

A solution comprising 0.49 grams potassium hydroxide, 40 grams of 4-acetoxystyrene, and 100 grams of absolute ethanol was refluxed for 4 hours. The reaction solution was cooled to 28° C. and 13 grams of potassium hydroxide pellets were added over a period of 10 minutes. After an additional 30 minutes of reaction, 64 grams di-tertiary-butyl-dicarbonate was charged portionwise over 20 minutes and the reaction was stirred for an additional hour at 28° C. After aqueous washing, the reaction product was extracted with ethyl acetate. The ethyl acetate was stripped from the extraction mixture on a rotary evaporator and the residual oil was charged with 0.07 grams phenothiazine. Distillation at 0.1 mm Hg gave 34.2 grams (64%) 4-tertiary-butoxycarbonyloxystyrene.

1. temperaturewas refluxed for 4 hours
2. additionwas charged portionwise over 20 minutes
3. extractionAfter aqueous washing, the reaction product was extracted with ethyl acetate
4. customThe ethyl acetate was stripped from the extraction mixture on a rotary evaporator
5. additionthe residual oil was charged with 0.07 grams phenothiazine
6. distillationDistillation at 0.1 mm Hg