HRID407120

反应详情

EQUATION

反应方程式

HRID 407120 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 500 g of 3,4-dimethoxybenzaldehyde in 2.5 L of methanol was added dropwise 529 g of bromine at room temperature (under cooling, if necessary) over 1 hour, and the mixture was stirred at the same temperature for 3 hours. To the reaction solution was added dropwise 2.5 L of water, and the crystals were precipitated. To the crystal suspension was added 20% aqueous sodium hydroxide solution at room temperature to adjust it to pH about 9 to 10, and then cooled. The precipitated crystals were collected by filtration and washed with water, and then dried at 50° C. for 12 hours to give 718.78 g of 6-bromo-3,4-dimethoxybenzaldehyde (yield: 98%).

WORKUP

后处理

  1. temperature(under cooling, if necessary) over 1 hour
  2. customthe crystals were precipitated
  3. additionTo the crystal suspension was added 20% aqueous sodium hydroxide solution at room temperature
  4. temperaturecooled
  5. filtrationThe precipitated crystals were collected by filtration
  6. washwashed with water
  7. customdried at 50° C. for 12 hours