HRID979976

反应详情

EQUATION

反应方程式

HRID 979976 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Hydroxy-3-methoxy-6-nitrobenzaldehyde potassium salt was slurried in acetone (500 mL) containing potassium carbonate (50 g) and the suspension was treated with dimethylsulfate (18.5 mL) and heated to reflux for one hour. An additional aliquot (18.5 mL) of dimethylsulfate was then added and the mixture was heated overnight. After 24 hours the red color of the potassium salt was virtually absent. The salts were removed by filtration, the filtrate was concentrated and the residue was recrystallized from isopropanol to give the title compound 40.0 g (80% from 3) mp 109°-110° C.

WORKUP

后处理

  1. temperatureheated
  2. temperatureto reflux for one hour
  3. temperaturethe mixture was heated overnight
  4. customThe salts were removed by filtration
  5. concentrationthe filtrate was concentrated
  6. customthe residue was recrystallized from isopropanol