HRID1288089

反应详情

EQUATION

反应方程式

HRID 1288089 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Dimethyl malonate (39.6 g) is added slowly with cooling and stirring to a solution of 6.9 g of sodium dissolved in 100 ml of absolute methanol and the mixture stirred for 15 min. The bromoester of formula 9, methyl cis-7-bromo-5-heptenoate (65.7 g) is added dropwise. The mixture is heated at reflux for 1 hr., cooled and diluted with water. The mixture is extracted with ether. The ether extracts are dried (Na2SO4) and concentrated. The residue is distilled under reduced pressure to give the title compound, b.p. 140° - 150° C/0.7 mm.

WORKUP

后处理

  1. temperaturewith cooling
  2. temperatureThe mixture is heated
  3. temperatureat reflux for 1 hr
  4. temperature, cooled
  5. extractionThe mixture is extracted with ether
  6. dry with materialThe ether extracts are dried (Na2SO4)
  7. concentrationconcentrated
  8. distillationThe residue is distilled under reduced pressure