反应详情

温度

0 °C

Thionyl chloride (0.295 mL, 4.04 mmol) was added to a suspension of ((2-((4-(difluoromethoxy)phenyl)amino)-4-methoxypyrimidin-5-yl)methanol (0.3 g, 1.009 mmol) in DCM (10 mL) cooled to 0° C. The mixture was stirred for 18 h while warming to room temperature. The reaction mixture was concentrated and dried under vacuum to give 5-(chloromethyl)-N-(4-(difluoromethoxy)phenyl)-4-methoxypyrimidin-2-amine hydrochloride as a beige solid (0.35 g, 97%). 1H NMR (400 MHz, DMSO-d6) δ ppm 9.98 (s, 1H), 8.34 (s, 1H), 7.87-7.72 (m, 2H), 7.42-6.86 (m, 3H), 4.67 (s, 2H), 4.02 (s, 3H).

1. temperaturewhile warming to room temperature
2. concentrationThe reaction mixture was concentrated
3. customdried under vacuum