反应详情

A solution of 303 g (1.14 mol) of 11-bromoundecanoic acid and 303 g (1.16 mol) of triphenylphosphine in 3L of toluene was stirred and refluxed under N2 for three days, then cooled to 0°. The crystalline solid was broken up, filtered off, washed with toluene and with ether, and then dissolved in a minimum of CH2Cl2. This solution was diluted with stirring to 4 L with ether, the white crystalline powder was filtered off and dried at 40°/1 ml; 524 g (87%), mp 95-98° . Calculated for C29H36 BrO2P: C, 66.03; H, 6.88. Found: C,66.36; H, 6.95.

1. temperaturerefluxed under N2 for three days
2. temperaturecooled to 0°
3. filtrationfiltered off
4. washwashed with toluene and with ether
5. dissolutiondissolved in a minimum of CH2Cl2
6. additionThis solution was diluted
7. filtrationthe white crystalline powder was filtered off
8. customdried at 40°/1 ml