HRID483714

反应详情

EQUATION

反应方程式

HRID 483714 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 3 g (9.4 mmol) of 4-cyanobenzyl 5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthyl ether in 60 ml of ether was added dropwise under nitrogen to a suspension of 1 g (26 mmol) of lithium aluminum hydride in 50 ml of dry ether at 25° C. The mixture was then stirred under reflux for 3 h, cooled and hydrolyzed cautiously with water and sodium sulfate solution. The mixture was extracted three times with ether, and the combined ether extracts were washed with water, dried over Na2SO4 and concentrated. 3 g of the title compound of melting point 77°-79° C. remained.

WORKUP

后处理

  1. temperatureunder reflux for 3 h
  2. temperaturecooled
  3. extractionThe mixture was extracted three times with ether
  4. washthe combined ether extracts were washed with water
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated