HRID1032485

反应详情

EQUATION

反应方程式

HRID 1032485 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 5.38 g (20 mmol) of N-benzyl-5,6-dimethoxyisoindoline, 50 ml of 48% hydrobromic acid was added, and the mixture was heated at reflux for 5 hours at an external temperature of from 110° to 125° C. After cooling, the precipitated crystals were collected by filtration and washed with 5 ml of water and 10 ml of acetone to obtain 6.36 g of the above identified compound as a grayish white powder. The powder was dissolved in 150 ml of hot water, and the solution was subjected to decolorization with 1.0 g of active carbon and then cooled with ice to obtain 4.75 g of prism crystals.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 5 hours at an external temperature of from 110° to 125° C
  3. temperatureAfter cooling
  4. filtrationthe precipitated crystals were collected by filtration
  5. washwashed with 5 ml of water and 10 ml of acetone
  6. customto obtain 6.36 g of the
  7. temperaturecooled with ice
  8. customto obtain 4.75 g of prism crystals