HRID2305950

反应详情

EQUATION

反应方程式

HRID 2305950 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
125 °C

PROCEDURE

实验过程

A 600 ml autoclave containing a mixture of 1-ethenyl-cyclopentanol (172.0 g; 1.54 mol), isopropenyl methyl ether (218.8 g; 3.04 mol), triethylamine (1.65 ml) and 85% H3PO4 (0.72 ml) was pressurized with N2 at 2 bar and heated up to 125° C. An increase of the pressure to 7 bar was observed. After 14 hours stirring, the autoclave was cooled down to room temperature and depressurized. MTBE (1.5 l) was added to the mixture, washed with H2O (4×25 ml) until neutral pH, dried (MgSO4) and concentrated. Distillation (61° C./0.1 torr) yielded 161.3 g (69% yield) of 5-cyclopentylidenepentan-2-one.

WORKUP

后处理

  1. additionA 600 ml autoclave containing
  2. temperatureAn increase of the pressure to 7 bar
  3. temperaturethe autoclave was cooled down to room temperature
  4. washwashed with H2O (4×25 ml) until neutral pH
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated
  7. distillationDistillation (61° C./0.1 torr)