HRID1816672

反应详情

EQUATION

反应方程式

HRID 1816672 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-Chloro-2-hydroxymethyl-3-methoxypyridine (41.0 g) was dissolved in methylene chloride (150 mL), and thionyl chloride was added dropwise over 10 minutes with stirring under cooling with an ice bath. The ice bath was removed, and the mixture was stirred for 30 minutes at room temperature. The solvent was removed under reduced pressure, and hexane (50 mL) was added to the residue, followed by distillation, whereby 4-chloro-2-chloromethyl-3-methoxypyridine chloride was obtained as a brown solid (54.1 g, yield: quantitative).

WORKUP

后处理

  1. temperatureunder cooling with an ice bath
  2. customThe ice bath was removed
  3. stirringthe mixture was stirred for 30 minutes at room temperature
  4. customThe solvent was removed under reduced pressure, and hexane (50 mL)
  5. additionwas added to the residue
  6. distillationfollowed by distillation