HRID1793651

反应详情

EQUATION

反应方程式

HRID 1793651 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 1000 ml round-bottom flask is loaded with 67 g (0.319 mol) of 2-hydroxymethyl-3-methoxy-4-chloro-pyridine hydrochloride and 469 ml of toluene. 73 g (0.606 mol) of thionyl chloride are then dropped therein, under stirring and at inner temperature of about 15–25° C. After completion of the addition, the mixture is washed with 35 ml of toluene, keeping the suspension at this temperature for at least 1 hour. After completion of the reaction, approx. 200 ml of solvent are distilled off under vacuum. The suspension, containing 2-chloromethyl-3-methoxy-4-chloro-pyridine, is then subjected to the subsequent step.

WORKUP

后处理

  1. additionAfter completion of the addition
  2. washthe mixture is washed with 35 ml of toluene
  3. customfor at least 1 hour
  4. customAfter completion of the reaction, approx. 200 ml of solvent
  5. distillationare distilled off under vacuum
  6. additionThe suspension, containing 2-chloromethyl-3-methoxy-4-chloro-pyridine