反应详情

温度

10 °C

Under an atmosphere of argon, a solution of phosphorus tribromide (8.32 g, 30.7 mmol) in 27 ml of n-hexane was added in dropwise to a mixture of 3,7,11,15,19,23,27,31,35,39-decamethyl-2,6,10,14,18,22,26,30,34,38-tetracontadecaen-1-ol (40 g, 57.3 mmol) and pyridine (1.92 ml, 23.8 mmol) in 587 ml of n-hexane at the temperature below 10° C. The solution was stirred at 10° C. for an hour, allowed to warm slowly from 10° to 20° C., stirred at 20°-25° C. for an hour and poured into cracked ice with stirring. The resulting precipitate was filtered off and the filtrate was extracted with n-hexane. The organic layer was washed with 5% sodium bicarbonate aqueous solution, dried over anhydrous sodium sulfate, filtered and evaporated in vacuo to dryness to afford 39.5 g (90.4%) of the desired compound, as a yellow oil.

1. temperatureto warm slowly from 10° to 20° C.
2. stirringstirred at 20°-25° C. for an hour
3. additionpoured into cracked ice
4. stirringwith stirring
5. filtrationThe resulting precipitate was filtered off
6. extractionthe filtrate was extracted with n-hexane
7. washThe organic layer was washed with 5% sodium bicarbonate aqueous solution
8. dry with materialdried over anhydrous sodium sulfate
9. filtrationfiltered
10. customevaporated in vacuo to dryness