HRID1197364
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas heated
- temperatureto reflux, under a nitrogen atmosphere, for 4.25 hours
- customThe solvent was removed under reduced pressure and water (50 ml)
- additionwas added to the residue
- extractionThe resulting aqueous phase was extracted with diethyl ether
- washthe organic extracts were washed with water and brine
- dry with materialbefore drying over anhydrous magnesium sulphate and evaporation in vacuo