HRID1650056

反应详情

EQUATION

反应方程式

HRID 1650056 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 25 g. (0.138 mmole) of 2-(2-bromoethyl)-1,3-dioxolane and 36.2 g. (0.138 mmole) of triphenylphosphine in 30 ml. of toluene was heated at 100° C. for 18 hours. The reaction was cooled to yield two phases. The toluene phase was decanted and the oil remaining crystalized at -78° C. in ethyl acetate. Decantation of the ethyl acetate and warming of the crystals to room temperature gave an oil. The oil was dried under vacuum (0.05 torr) at 100° C. for 16 hours to yield 15 g. (27%) of the title compound as a solid glass which was ground to a powder.

WORKUP

后处理

  1. temperatureThe reaction was cooled
  2. customto yield two phases
  3. customThe toluene phase was decanted
  4. customthe oil remaining crystalized at -78° C. in ethyl acetate
  5. customgave an oil
  6. customThe oil was dried under vacuum (0.05 torr) at 100° C. for 16 hours
  7. customto yield 15 g