反应详情

温度

95 °C

A mixture of 2-fluoro-4-iodoaniline (24.19 g, 0.100 mole) and potassium ethylxanthogenate (35.27 g, 0.220 mole) in N,N-dimethylformamide (80 mL) was stirred at 95° C. for 5 hours. The reaction mixture was cooled to room temperature then diluted with water (150 mL) and 1 N aqueous HCl (200 mL). The mixture was stirred at room temperature overnight. The resulting precipitate was collected by filtration and rinsed with water. The solid was dried overnight at 85° C. in a vacuum oven to provide 6-iodobenzo[d]thiazole-2-thiol. 1H NMR (300 MHz, CD3OD) δ ppm 7.09 (d, J=8 Hz, 1H), 7.70 (dd, J=2, 8 Hz, 1H), 8.10 (d, J=2 Hz, 1H), 13.82 (Sbroad, 1H); MS (DCI/NH3) m/z 294 (M+H)+.

1. temperatureThe reaction mixture was cooled to room temperature
2. stirringThe mixture was stirred at room temperature overnight
3. filtrationThe resulting precipitate was collected by filtration
4. washrinsed with water
5. customThe solid was dried overnight at 85° C. in a vacuum oven