反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
Acetyl chloride (2.75 g) was mixed with acetonitrile (70 ml), and the mixture was cooled to 0° C. Then, potassium thiocyanate (3.75 g) was added thereto, and the mixture was stirred at room temperature for 6 hours. After cooling to 0° C. again, 3-trifluoromethyl-N-propargyl-aniline (7 g) was added thereto, and the mixture was stirred at room temperature for 3 hours. After the solvent was distilled off under reduced pressure, the residue was extracted with ethyl acetate (300 ml), and the extract was washed with water. The solvent was distilled off to give N-[3-(trifluoromethyl)phenyl]-N-propargyl-N'-acetylthiourea as crystallines (8 g). This identification was achieved by proton nuclear magnetic resonance (1H-NMR).
WORKUP
后处理
- temperatureAfter cooling to 0° C. again
- stirringthe mixture was stirred at room temperature for 3 hours
- distillationAfter the solvent was distilled off under reduced pressure
- extractionthe residue was extracted with ethyl acetate (300 ml)
- washthe extract was washed with water
- distillationThe solvent was distilled off