HRID1976521

反应详情

EQUATION

反应方程式

HRID 1976521 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 40.0 g (268.1 mol) of m-acetotoluidine, 45.0 g (223.9 mol) of 3,4-bromomethylenedioxybenzene, 8 g (50.1 mol) of copper sulfate, and 31 g (267.7 mmol) of potassium carbonate was reacted in the same manner as in Example 5 (2) to obtain a crude reaction product. A mixture of this crude product, 50 g (757.4 mmol) of 85% KOH, and 200 ml of methanol was refluxed overnight and then concentrated. Water was added thereto. The resultant mixture was extracted with toluene twice. The toluene phase was washed with water three times, dried, and then concentrated. The residue was distilled under vacuum to obtain 24.51 g of N-3,4-methylenedioxyphenyl-N-m-tolylamine.

WORKUP

后处理

  1. customto obtain a crude
  2. customreaction product
  3. temperaturewas refluxed overnight
  4. concentrationconcentrated
  5. additionWater was added
  6. extractionThe resultant mixture was extracted with toluene twice
  7. washThe toluene phase was washed with water three times
  8. customdried
  9. concentrationconcentrated
  10. distillationThe residue was distilled under vacuum