HRID1197364

反应详情

EQUATION

反应方程式

HRID 1197364 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-methyl-2-(pent-4-ynyl)malonic acid (5.7 g) and cuprous oxide (0.22 g) in acetonitrile (150 ml) was heated to reflux, under a nitrogen atmosphere, for 4.25 hours. The solvent was removed under reduced pressure and water (50 ml) was added to the residue followed by sufficient concentrated hydrochloric acid to hydrolyse the copper salts. The resulting aqueous phase was extracted with diethyl ether and the organic extracts were washed with water and brine before drying over anhydrous magnesium sulphate and evaporation in vacuo. 2-Methylhept-6-ynoic acid (3.6 g) was obtained as a colourless oil after distillation (b.p. 150°-165°, 0.5 mm Hg).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureto reflux, under a nitrogen atmosphere, for 4.25 hours
  3. customThe solvent was removed under reduced pressure and water (50 ml)
  4. additionwas added to the residue
  5. extractionThe resulting aqueous phase was extracted with diethyl ether
  6. washthe organic extracts were washed with water and brine
  7. dry with materialbefore drying over anhydrous magnesium sulphate and evaporation in vacuo