HRID1471381

反应详情

EQUATION

反应方程式

HRID 1471381 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

In an autoclave under N2, a mixture of 1-vinylcyclopentanol (65 g, 0.58 mol), 2-methoxypropene (108 ml, 1.15 mol), 85% phosphoric acid (0.29 ml), triethylamine (0.63 ml) was heated at 130° C. for 15 h. The reaction mixture was cooled to 20° C., diluted with MTBE (500 ml), washed three times with water (25 ml), once with a saturated aqueous solution of NaCl (25 ml), dried (MgSO4) and concentrated. Widmer-Distillation (0.13 mbar, head temp. 58° C.) of the crude product gave 5-cyclopentylidenepentan-2-one (63.67 g, 72%).

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to 20° C.
  2. washwashed three times with water (25 ml)
  3. dry with materialonce with a saturated aqueous solution of NaCl (25 ml), dried (MgSO4)
  4. concentrationconcentrated
  5. distillationWidmer-Distillation (0.13 mbar, head temp. 58° C.) of the crude product