HRID1614067

反应详情

EQUATION

反应方程式

HRID 1614067 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
45 °C

PROCEDURE

实验过程

To a solution of 3-cyclopenten-1-ol (15.3 g), N-hydroxyphthalimide (29.7 g) and triphenylphosphine (47.7 g) in tetrahydrofuran (250 ml) was added diethyl azodicarboxylate (31.7 g) at 40° to 50° C. After stirring at 45° C. for 2 hours, the reaction mixture was poured into ice-water and extracted with ethyl acetate. The separated organic layer was washed with 5% aqueous solution of sodium bicarbonate, brine, successively and dried over magnesium sulfate. The solvent was evaporated in vacuo, and the residual oil was subjected to column chromatography on silica gel. The desired product was eluted with 15% ethyl acetate in n-hexane to give N-(3-cyclopenten-1-yloxy)phthalimide (25.6 g).

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. washThe separated organic layer was washed with 5% aqueous solution of sodium bicarbonate, brine
  3. dry with materialsuccessively and dried over magnesium sulfate
  4. customThe solvent was evaporated in vacuo
  5. washThe desired product was eluted with 15% ethyl acetate in n-hexane