反応 #5422

反応方程式

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

n-butyl chlorocarbonate

triethylamine

→

2-butoxycarbonylimino-3-(3-trifluoromethylphenyl)thiazolidine

収率 40.5%

溶媒

tetrahydrofuran

反応条件

後処理

1. 1
   その他The solvent was removed
2. 2
   抽出the residue was extracted with ethyl acetate
3. 3
   洗浄washed with water
4. 4
   乾燥dried over anhydrous magnesium sulfate
5. 5
   その他After removal of the solvent

実験手順

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.

出典