반응 #727206

반응 방정식

Tetra-n-butylammonium di-tert-butyl phosphate

1,2-dibromoethane

→

2-bromoethyl di-tert-butyl phosphate

수율 46.2%

용매

dimethoxyethane

반응 조건

후처리

1. 1
   온도refluxed for 4 hr
2. 2
   여과filtered
3. 3
   농축The filtrate was concentrated
4. 4
   workup.ADDITIONdiluted with diethyl ether
5. 5
   세척washed with 20% aqueous potassium carbonate solution
6. 6
   건조dried over magnesium sulphate
7. 7
   기타evaporated
8. 8
   기타to leave a colourless oil
9. 9
   기타The crude product was purified by silica gel chromatography
10. 10
    세척eluting with a 20-50% mixture of ethyl acetate in iso-hexane

실험 절차

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:

출처