반응 #50317

반응 방정식

N-(3-trifluoromethylphenyl)thiourea

dibromoethane

potassium carbonate

→

2-imino-3-(3-trifluoromethylphenyl)thiazolidine

수율 110.0%

용매

acetone

반응 조건

후처리

1. 1
   기타The solvent was removed by distillation
2. 2
   추출the residue was extracted with ethyl ether
3. 3
   세척washed with water
4. 4
   건조dried over anhydrous magnesium sulfate

실험 절차

A solution of N-(3-trifluoromethylphenyl)thiourea (6.1 g) , dibromoethane (5.7 g) and anhydrous potassium carbonate (11.5 g) in acetone (60 ml) was refluxed for 1 day. The solvent was removed by distillation therefrom, and the residue was extracted with ethyl ether, washed with water, dried over anhydrous magnesium sulfate and subjected to column chromatography to give 7.5 g of 2-imino-3-(3-trifluoromethylphenyl)thiazolidine. The thus obtained 2-imino-3- (3-trifluoromethylphenyl) thiazolidine (1.0 g), n-butyl chlorocarbonate (0.61 g) and triethylamine (1.2 g) were dissolved in tetrahydrofuran, and the resultant solution was stirred at room temperature for 5 hours. The solvent was removed, and the residue was extracted with ethyl acetate, washed with water and dried over anhydrous magnesium sulfate. After removal of the solvent, the residue was subjected to column chromatography to give 0.57 g of 2-butoxycarbonylimino-3- (3-trifluoromethylphenyl) thiazolidine.

출처