反应详情

4-Dimethylaminomethyl-2-hydroxymethylpyridine (13.45 g) in dichloromethane (200 ml) was added dropwise to a stirred solution of thionyl chloride (30 ml) in dichoromethane (150 ml). The resulting red mixture was stirred for 1 hour then concentrated in vacuo. The residue was treated with ether (300 ml) to yield a crystalline solid. Recrystallisation from methanol/ether (1:3) yielded 2-chloromethyl-4-dimethylaminomethylpyridine dihydrochloride (20.04 g) as an orange solid m.p. 202°-204°.

1. concentrationthen concentrated in vacuo
2. additionThe residue was treated with ether (300 ml)
3. customto yield a crystalline solid
4. customRecrystallisation from methanol/ether (1:3)