HRID267303

反应详情

EQUATION

反应方程式

HRID 267303 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-chloro-2-(pent-2-ynyl)-cyclohexane-1,3-dione (80 g; 0.377 Mole) in dry xylene (800 ml) was allowed to reflux in the presence of anhydrous sodium carbonate (39.2 g; 0.38 Mole) until gas evolution ceased (12 h.). The reaction mixture was cooled, washed three times with water, and dried over magnesium sulfate, and the xylene was removed in vacuo. The resulting residue was distilled through a Vigreux column to afford 2-(pent-2-ynyl)-cyclopent-2-enone (41.3 g; 74 % yield), b.p. 67°-8°/0.01 Torr.

WORKUP

后处理

  1. custom(12 h.)
  2. temperatureThe reaction mixture was cooled
  3. washwashed three times with water
  4. dry with materialdried over magnesium sulfate
  5. customthe xylene was removed in vacuo
  6. distillationThe resulting residue was distilled through a Vigreux column