HRID1417520

反应详情

EQUATION

反应方程式

HRID 1417520 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

A mixture of 272 ml of toluene and 199.5 g benzylamine was prepared and heated to 90° C. The chlorindan was added dropwise to the mixture over a 30 minute period. The reaction mixture was heated to 115° C. for ten hours. The reaction mixture was cooled to ambient temperature and 300 ml of water was added. The resulting heterogeneous mixture was then brought to pH2.2 by the addition of 33% H2SO4. The phases were separated and the organic layer discarded. The pH of the aqueous layer was adjusted to pH6.0 prior to extraction with 300 ml of toluene. A further 100 ml of toluene was then added and the aqueous phase discarded. The toluene was removed under vacuo from the combined organic layer leaving 104.3 g racemic N-benzyl-1-aminoindan base as an oil (72.5% yield).

WORKUP

后处理

  1. customwas prepared
  2. temperatureThe reaction mixture was heated to 115° C. for ten hours
  3. temperatureThe reaction mixture was cooled to ambient temperature
  4. customThe phases were separated
  5. extractionto extraction with 300 ml of toluene
  6. additionA further 100 ml of toluene was then added
  7. customThe toluene was removed under vacuo from the combined organic layer