HRID2232464

反应详情

EQUATION

反应方程式

HRID 2232464 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

4.6 g of 4,4-dimethyl-6-(1-bromoethyl)chromane were dissolved in 40 ml of xylene and the solution was treated with 5.3 g of triphenylphosphine. The mixture was heated to 100° C. overnight, cooled, the precipitated crystals were filtered off under suction and washed with hexane. For the further purification, the phosphonium salt was dissolved in methylene chloride and precipitated again by the addition of ethyl acetate. There were obtained 3.5 g of [1-(4,4-dimethyl-6-chromanyl)ethyl]triphenylphosphonium bromide in the form of colorless crystals of melting point 142°-148° C.

WORKUP

后处理

  1. temperaturecooled
  2. filtrationthe precipitated crystals were filtered off under suction
  3. washwashed with hexane
  4. customFor the further purification
  5. dissolutionthe phosphonium salt was dissolved in methylene chloride
  6. customprecipitated again by the addition of ethyl acetate