HRID463044
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
6-Bromo-2,2-dimethylhexanoic acid (3.8 g, 17 mmole) and triphenylphosphine (4.9 g, 18.7 mmole) were dissolved in acetonitrile (30 ml), and the solution was heated under reflux for 20 hours. After the completion of the reaction, the solvent was removed under reduced pressure, and the residue was treated with toluene, followed by thorough stirring. The insolubles were seperated from the toluene solution, and crystallized from ethyl acetate to give 5-carboxy-5,5-dimethylpentyltriphenylphosphonium bromide (4.8 g, 58%) [NMR (δ value): 1.10 (6H,s), 1.4-1.6 (6H), 3.4-3.8 (2H)].
WORKUP
后处理
- temperaturethe solution was heated
- temperatureunder reflux for 20 hours
- customAfter the completion of the reaction
- customthe solvent was removed under reduced pressure
- additionthe residue was treated with toluene
- customThe insolubles were seperated from the toluene solution
- customcrystallized from ethyl acetate