반응 #6455

반응 방정식

sodium bicarbonate

5-methylisatin

sodium hydride

acetic anhydride

→

1-acetyl-5-methylisatin

수율 47.6%

용매

toluene

반응 조건

후처리

1. 1
   workup.STIRRINGWhile stirring under ice cooling
2. 2
   온도by heating at 80° C. for further an hour
3. 3
   workup.STIRRINGwith stirring
4. 4
   기타After completion of the reaction
5. 5
   여과The crystals were filtered
6. 6
   세척washed with water
7. 7
   기타dried

실험 절차

With stirring at 0° C., 8.06 g (50.0 mmols) of 5-methylisatin was added by small portions to a solution of 2.00 g (50.0 mmols) of sodium hydride in toluene. While stirring under ice cooling, 4.7 ml (50.0 mmols) of acetic anhydride was dropwise added to the mixture followed by heating at 80° C. for further an hour with stirring. After completion of the reaction, an aqueous saturated sodium bicarbonate solution was added to the reaction mixture. The crystals were filtered, washed with water and dried to give 4.84 g (yield, 47%) of 1-acetyl-5-methylisatin.

출처