HRID66635

反应详情

EQUATION

反应方程式

HRID 66635 的结构方程式

PROCEDURE

实验过程

Thionyl chloride (288 g) is added over 1.5 hour to a stirred solution of 2,3-dimethoxybenzyl alcohol (400 g) and 2,6-lutidine in methylene chloride (2 l). The reaction mixture is then stirred for 30 minutes after which it is washed with 2 N hydrochloric acid (7×1 l) and then with water. The organic layer is separated, dried (MgSO4) and evaporated to give a residue, which upon distillation yields 3,4-dimethoxybenzyl chloride (375 g), b.p. 145°-150° C. at 20-25 nm (waterpump vacuum). The material solidifies on standing.

WORKUP

后处理

  1. washis washed with 2 N hydrochloric acid (7×1 l)
  2. customThe organic layer is separated
  3. dry with materialdried (MgSO4)
  4. customevaporated
  5. customto give a residue, which
  6. distillationupon distillation