反应详情

To 40 ml of concentrated sulfuric acid with stirring under ice-cooling is added a mixture of 10 g of 4'-hydroxypropiophenone and 10 g of N-hydroxymethylchloroacetic amide in a small portion. After addition, the reaction mixture is further stirred under ice-cooling for 130 minutes. The resulting mixture is poured into ice-cold water containing sodium chloride and the solution is extracted with ethyl acetate. The ethyl acetate layer is washed with water and dried over sodium sulfate and then filtered. The filtrate is concentrated under reduced pressure and obtained white crystals are recrystallized from a mixture of hexane and ethanol to give 9.6 g of 3'-chloroacetamidomethyl-4'-hydroxypropiophenone as white crystals, melting at 143°-145° C.

1. temperaturecooling
2. additionis added
3. additionAfter addition
4. temperaturecooling for 130 minutes
5. additionThe resulting mixture is poured into ice-cold water
6. extractionthe solution is extracted with ethyl acetate
7. washThe ethyl acetate layer is washed with water
8. dry with materialdried over sodium sulfate
9. filtrationfiltered
10. concentrationThe filtrate is concentrated under reduced pressure
11. customobtained white crystals
12. customare recrystallized from a mixture of hexane and ethanol