HRID1650056
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe reaction was cooled
- customto yield two phases
- customThe toluene phase was decanted
- customthe oil remaining crystalized at -78° C. in ethyl acetate
- customgave an oil
- customThe oil was dried under vacuum (0.05 torr) at 100° C. for 16 hours
- customto yield 15 g