反应详情

温度

60 °C

A solution of 2-imino-3-(3-trifluoromethylphenyl)-5-methylthiazoline hydrochloride (1.47 g, 5.0 mmol) and morpholine (1.57 g, 18.0 mmol) in N,N-dimethylformamide (10 ml) charged in a reaction flask was reacted with tetrafluoroethylene, which was made to flow intothe flask (ca. 0.7 liter/hr), with vigorous stirring at 60° C. for 2 hours. After cooling to an ambient temperature, the reaction mixture was poured into saturated aqueous sodium hydrogencarbonate solution (100 ml), and extracted twice with toluene (100 ml×2). The toluene layer was washed twice with 5% hydrochloric acid (50 ml×2) and water (70 ml) and then brine (70 ml), and dried over anhydrous magnesium sulfate. The solvent was distilled off, and the residue was subjected to silica gel column chromatography, which afforded 2-difluoroacetylimino-3-(3-trifluoromethylphenyl)-5-methylthiazoline (1.47 g, 4.4 mmol, yield 87%).

1. customto flow intothe flask
2. temperatureAfter cooling to an ambient temperature
3. extractionextracted twice with toluene (100 ml×2)
4. washThe toluene layer was washed twice with 5% hydrochloric acid (50 ml×2) and water (70 ml)
5. dry with materialbrine (70 ml), and dried over anhydrous magnesium sulfate
6. distillationThe solvent was distilled off