HRID261206

反应详情

EQUATION

反应方程式

HRID 261206 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 43 g of 6-chloro-3a,4,9,9a-tetrahydro-2-methylbenz[f]isoindolin-4-one in 430 ml of tetrahydrofuran is added dropwise at room temperature with stirring to 170 ml of a ca. 5% solution of methyl lithium in ether in a nitrogen atmosphere and the mixture is stirred for 51/2 hours at room temperature. Thereafter, saturated ammonium chloride solution and water are added and the mixture extracted with methylene chloride. The organic phase is dried over sodium sulphate and evaporated. The residue is crystallised from ether/petroleum ether to yield 6-chloro-3a,4,9,9a-tetrahydro-2,4-dimethylbenz[f]-isoindolin-4-ol. M.P. 125°-130°.

WORKUP

后处理

  1. extractionthe mixture extracted with methylene chloride
  2. dry with materialThe organic phase is dried over sodium sulphate
  3. customevaporated
  4. customThe residue is crystallised from ether/petroleum ether