HRID372542

反应详情

EQUATION

反应方程式

HRID 372542 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 11.2 g of 7-dimethylamino-6,7-dihydro [5H] benzocycloheptene, 800 ml of ethanol and 11.2 g carbon containing 10% of Pd (OH)2 was held under a hydrogen atmosphere for 30 minutes and when the theoretical amount of hydrogen had been absorbed, the mixture was filtered. The filtrate was evaporated to dryness and the residue was chromatographed over silica gel. Elution with an 8-2-1 ethyl acetate-benzene-triethylamine mixture yielded 4.1 g of 7-dimethylamino-6,7,8,9-tetrahydro [5H] benzocycloheptene.

WORKUP

后处理

  1. customwhen the theoretical amount of hydrogen had been absorbed
  2. filtrationthe mixture was filtered
  3. customThe filtrate was evaporated to dryness
  4. customthe residue was chromatographed over silica gel
  5. washElution with an 8-2-1 ethyl acetate-benzene-triethylamine mixture