反应详情

A mixture of 10 ml (75 mmol) of 6-chlorohexanol and 16.9 g (112 mmole) of Nal dissolved in 100 ml acetone was refluxed for 3.5 days. The reaction mixture was filtered and the filtrate was concentrated to an oil and dissolved in 100 ml of ether. The ether solution was filtered, concentrated to an oil, and dissolved in 30 ml of diethylamine. The solution was stirred for 4 hours and filtered. The filtrate was concentrated to an oil, taken up in acidified water (pH<2) and washed with ethylacetate. The acidic solution was then adjusted to pH 9.5 and extracted twice with ethyl acetate. The organic extract was dried over MgSO4 and concentrated under vacuum to yield 7.5 g of the title compound as an oily product.

1. temperaturewas refluxed for 3.5 days
2. filtrationThe reaction mixture was filtered
3. concentrationthe filtrate was concentrated to an oil
4. dissolutiondissolved in 100 ml of ether
5. filtrationThe ether solution was filtered
6. concentrationconcentrated to an oil
7. dissolutiondissolved in 30 ml of diethylamine
8. filtrationfiltered
9. concentrationThe filtrate was concentrated to an oil
10. washwashed with ethylacetate
11. extractionextracted twice with ethyl acetate
12. extractionThe organic extract
13. dry with materialwas dried over MgSO4
14. concentrationconcentrated under vacuum