HRID1607627

反应详情

EQUATION

反应方程式

HRID 1607627 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In 40 ml of 5% sodium hydroxide solution 3.84 g (20 millimoles) of 7-hydroxy-2,2-dimethyl-4-chromanone are dissolved whereupon 80 ml of dichloro methane and 0.5 g of triethyl benzyl ammonium chloride are added and the mixture is intensively stirred at room temperature for 20 minutes. After addition of 4.25 g (1.9 ml, 30 millimole) of methyl iodide the reaction mixture is stirred for 2 hours. The organic layer is separated, washed twice with 50 ml of water each, dried over sodium sulfate and evaporated. The residue is crystallized from 80% methanol. Thus 3.9 g of the desired compound are obtained, yield 94.6%. Mp.: 77°-78° C.

WORKUP

后处理

  1. additionare added
  2. stirringis stirred for 2 hours
  3. customThe organic layer is separated
  4. washwashed twice with 50 ml of water each,
  5. dry with materialdried over sodium sulfate
  6. customevaporated
  7. customThe residue is crystallized from 80% methanol