HRID1927644
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
To a mixture of 4,4-dimethyl-1-pentene (10 g), acetone (600 mL), water (140 mL) and acetic acid (13.5 mL) at rt was added a solution of potassium permanganate (22.3 g) in water (85 mL), followed by additional acetone (270 mL). After stirring for 40 min, sodium nitrite (11.7 g) was added, followed by dilute sulfuric acid (12%, 221 mL). The product was extracted with ether:hexanes (1:1), and the extracts were washed with saturated sodium bicarbonate and brine, dried (sodium sulfate) and concentrated. The resulting residue was purified on silica gel column (5-100% ether in hexanes) to give the title compound.
WORKUP
后处理
- extractionThe product was extracted with ether:hexanes (1:1)
- washthe extracts were washed with saturated sodium bicarbonate and brine
- dry with materialdried (sodium sulfate)
- concentrationconcentrated
- customThe resulting residue was purified on silica gel column (5-100% ether in hexanes)