HRID1586899

反应详情

EQUATION

反应方程式

HRID 1586899 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
170 °C

PROCEDURE

实验过程

Ethyl 3-acetoxyacrylate (1, 11.0 g, 69.6 mmol) and butadiene (30.0 ml, 0.8 mol) were dissolved in toluene (distilled from calcium hydride, 25 ml); the mixture was placed in a 500 ml autoclave at -78° C. The autoclave was sealed, and then heated for 15 hours at 170° C. The autoclave was cooled and opened, the contents centrifuged, and the gummy residue extracted with toluene (3×100 ml). The toluene was removed under vacuum, and the mixture of cis and trans 1-acetoxy-2-carboethoxycyclohex-4-ene (3 and 2) was isolated by distillation (101° C. at 2 torr).

WORKUP

后处理

  1. customwas placed in a 500 ml autoclave at -78° C
  2. customThe autoclave was sealed
  3. temperatureThe autoclave was cooled
  4. extractionthe gummy residue extracted with toluene (3×100 ml)
  5. customThe toluene was removed under vacuum
  6. additionthe mixture of cis