反応 #524229

反応方程式

diethylphosphite

diethylphosphite

isobutene

ditertiarybutyl peroxide

→

pure product

収率 81.0%

isobutanephosphonic acid diethyl ester

収率 81.0%

反応条件

後処理

1. 1
   workup.ADDITIONis added drop by drop
2. 2
   温度The reaction heat that
3. 3
   その他develops is removed by external cooling
4. 4
   温度Then heating at 150° C.
5. 5
   workup.DISTILLATIONVacuum distillation through a 12-tray column

実験手順

In a 10-liter flask with stirrer, internal thermometer, reflux condenser (-80° C.) and a cooled dropping funnel, 2070 g of diethylphosphite is heated to 150° C. Then over a period of about 90 minutes a mixture of 2070 g of diethylphosphite, 1680 g of isobutene and 44 g of ditertiarybutyl peroxide is added drop by drop. The reaction heat that develops is removed by external cooling. Then heating at 150° C. continues for about 30 minutes. Vacuum distillation through a 12-tray column delivers an 81% yield of pure product.

出典