反应详情

Tetra-n-butylammonium di-tert-butyl phosphate (4.0 g, 8.87 mmol) and 1,2-dibromoethane (5.0 g, 26.7 mmol) in dimethoxyethane (20 ml) were stirred and refluxed for 4 hr. then cooled to room temperature and filtered. The filtrate was concentrated, diluted with diethyl ether, washed with 20% aqueous potassium carbonate solution, dried over magnesium sulphate and evaporated to leave a colourless oil. The crude product was purified by silica gel chromatography eluting with a 20-50% mixture of ethyl acetate in iso-hexane to give 2-bromoethyl di-tert-butyl phosphate (1.3 g, 46% yield) as a colourless oil:

1. temperaturerefluxed for 4 hr
2. filtrationfiltered
3. concentrationThe filtrate was concentrated
4. additiondiluted with diethyl ether
5. washwashed with 20% aqueous potassium carbonate solution
6. dry with materialdried over magnesium sulphate
7. customevaporated
8. customto leave a colourless oil
9. customThe crude product was purified by silica gel chromatography
10. washeluting with a 20-50% mixture of ethyl acetate in iso-hexane