反应详情

To a solution of 4-chloro-2-hydroxymethyl-3,5-dimethylpyridine (60.7 g, 354 mmol) and DMF (0.25 mL, 3.54 mmol) in toluene (200 mL) was added thionyl chloride (26.9 mL, 371 mmol) over 2 h at 15-30° C. After stirring for 2 more h at ambient temperature, ethanol (6 mL) was added to the thick slurry. The solids were filtered off at about 10° C., washed with toluene (80 mL) and dried at 40° C. in vacuo to give 4-chloro-2-chloromethyl-3,5-dimethylpyridinium chloride as an off-white solid (m. p. 195-196° C.); yield 66.5 g (84%).

1. filtrationThe solids were filtered off at about 10° C.
2. washwashed with toluene (80 mL)
3. customdried at 40° C. in vacuo