HRID1966812

反应详情

EQUATION

反应方程式

HRID 1966812 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

Potassium tert-butoxide (3.230 gm, 28.812 mmol) and triphenylphosphine methyl iodide (10.286 gm, 28.812 mmol) were dissolved in dry tetrahydrofuran (30 ml). The mixture was cooled to −78° C. and stirred at the same temperature for about 15 minutes. 1,4-Dioxaspiro[4.5]decan-8-one (3.0 gm, 19.208 mmol) in tetrahydrofuran was added drop wise and the mixture was stirred at the same temperature for about 30 minutes and then it was warmed to room temperature and stirred overnight, extaction was done with ethyl acetate and water. The organic layer was dried over sodium sulphate and concentrated. Purification was done by column chromatography.

WORKUP

后处理

  1. stirringthe mixture was stirred at the same temperature for about 30 minutes
  2. temperatureit was warmed to room temperature
  3. stirringstirred overnight
  4. dry with materialThe organic layer was dried over sodium sulphate
  5. concentrationconcentrated
  6. customPurification