反应详情

温度

72 °C

4-bromo-2,6-difluorobenzenamine (2.514 g, 12.1 mmol) was dissolved in acetone (75 ml) and ethanoyl isothiocyanate (1.30 ml, 14.8 mmol) was added. The reaction flask was fit with a reflux condensor and placed in a preheated oil bath (70-74° C.) and the reaction was stirred under nitrogen for 90 minutes. The reaction was then cooled to room temperature and poured into water (200 ml), and the resultant suspension was filtered. The solid was washed with water, collected, and dried under high vacuum in water bath (60° C.) to afford 1-acetyl-3-(4-bromo-2,6-difluorophenyl)thiourea (3.435 g, 93% purity, 85% yield). MS (ESI pos. ion) m/z: 309 (MH+, 79Br), 311 (MH+, 81Br). Calculated exact mass for C9H7BrF2N2OS 308 (79Br), 310 (81Br).

1. customplaced in a preheated oil bath
2. temperatureThe reaction was then cooled to room temperature
3. filtrationthe resultant suspension was filtered
4. washThe solid was washed with water
5. customcollected
6. dry with materialdried under high vacuum in water bath (60° C.)