反应详情

To a solution of 18.9 g of 4-carboxybenzalacetophenone in 7.5 ml of 1N sodium hydroxide solution and 225 ml of water was added 15 ml of 30% hydrogen peroxide. After cooling in an ice-water bath, 50 ml of 0.5N sodium hydroxide was added dropwise over 5 min. The reaction mixture was stirred at room temperature for 31/4 hrs. and acidified to pH of 6.5 with 1N hydrochloric acid. After stirring at room temperature for 1 hr., the solid was collected on a filter, washed with water and air-dried. Recrystallization from ethanol gave 11 g of 3-(4-carboxyphenyl)-1-phenyl-2,3-epoxy-1-propanone as colorless crystals, m.p. 170°-172° C. after drying at 80° C. under vacuum for 3 hrs.

1. temperatureAfter cooling in an ice-water bath
2. stirringAfter stirring at room temperature for 1 hr
3. custom, the solid was collected on a filter
4. washwashed with water
5. customair-dried
6. customRecrystallization from ethanol