반응 #317266

반응 방정식

thiobenzamide

1,3-dichloroacetone

→

4-chloromethyl-2-phenylthiazole

수율 57.0%

용매

methanol

반응 조건

후처리

1. 1
   온도under reflux for 1 hour
2. 2
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure, and ice water
3. 3
   workup.ADDITIONwas added to the remaining product, which
4. 4
   추출The resulting product was extracted with ethyl acetate
5. 5
   세척washed with saturated saline
6. 6
   건조dried over sodium sulfate
7. 7
   workup.DISTILLATIONthe solvent was distilled off under reduced pressure
8. 8
   기타The residual product was purified through silica gel column chromatography

실험 절차

2.33 g of thiobenzamide was dissolved in 20 ml of dry methanol, and 2.16 g of 1,3-dichloroacetone was added thereto at room temperature and then heated under reflux for 1 hour. The solvent was distilled off under reduced pressure, and ice water was added to the remaining product, which was then neutralized with an aqueous solution of sodium hydrogen carbonate. The resulting product was extracted with ethyl acetate, washed with saturated saline, and dried over sodium sulfate, and the solvent was distilled off under reduced pressure. The residual product was purified through silica gel column chromatography to obtain 2.03 g of 4-chloromethyl-2-phenylthiazole was obtained from the fraction eluted with chloroform/n-hexane=1/2.

출처