反应详情

A solution of thionyl chloride (4 ml) in dichloromethane (20 ml) is added dropwise to a solution of 3-chloro-4-[N-(2-hydroxyethyl)-N-methylamino]-2-hydroxymethylpyridine (2.3 g) in dichloromethane (30 ml) at 0° C. The temperature is then allowed to rise to 20° C. (20 min), and then the temperature is kept at 40° C. for 30 min. The solvent is stripped off in vacuo and then the remaining residue is chromatographed on silica gel (petroleum ether/ethyl acetate 7/3 mixture which contains 1 ml of conc. NH3 ×aq/l). Yield: 2.6 g.

1. customto rise to 20° C.
2. custom(20 min)
3. customthe remaining residue is chromatographed on silica gel (petroleum ether/ethyl acetate 7/3 mixture which contains 1 ml of conc. NH3 ×aq/l)