反应 #2383786
ord-94d63f3bf0544516b297b5d11806b7ff
反应方程式
溶剂
反应条件
后处理
- 1workup.ADDITIONwas added
- 2温度The obtained mixture was heated for 5 hours
- 3其他was simultaneously removed with Dean-Stark apparatus (Vogel's Textbook of Practical Organic Chemistry, Fourth Ed., Longman, London, 1978, p. 411)
- 4干燥The obtained solution was dried with magnesium sulfate
- 5过滤after the filtration of the drying agent hexane
- 6其他was evaporated
- 7workup.DISTILLATIONThe crude residue was distilled under reduced pressure 10 mbar at the temperature of 95° C.
实验过程
To a mixture of 4-chlorobutyric acid (48 ml; 0.48 mole), allyl alcohol (200 ml) and hexane (1.2 l) p-toluenesulfonic acid (16.0 g; 0.08 mole) was added. The obtained mixture was heated for 5 hours at reflux temperature in such a way that water was simultaneously removed with Dean-Stark apparatus (Vogel's Textbook of Practical Organic Chemistry, Fourth Ed., Longman, London, 1978, p. 411). The mixture was then cooled to room temperature and shaken with 7% aqueous sodium hydrogencarbonate solution (2×500 ml). The obtained solution was dried with magnesium sulfate and after the filtration of the drying agent hexane was evaporated. The crude residue was distilled under reduced pressure 10 mbar at the temperature of 95° C. and the title compound (61.2 g; 79%) was obtained in the form of a colourless oil.