反应详情

温度

60 °C

A thermostatically controllable reactor is charged with 553.8 g (2.1 mol) of (4-hydroxy-3,5-di-tert-butylbenzyl)dimethylamine und 450 g of petroleum ether 100/140. With stirring and blanketing with inert gas, the reaction mixture is heated to 60° C. and 366.4 g (2.2 mol) of triethyl phosphite are run into the clear solution. With cooling, 225.1 g (2.2 mol) of acetic anhydride are then added dropwise over 2 hours at 60° C., and stirring is continued for 1 hour at 60° C. The solvent is removed by distillation until the temperature is 115° C. The residual reaction solution is washed with 4×250 ml of water at 75° C. and dried by azeotropic distillation. Upon cooling to room temperature, the product crystallises and is filtered with suction, washed with petroleum ether 100/140 and dried, giving 693.2 g (92.6% of theory) of colourless diethyl 4-hydroxy-3,5-di-tert-butylbenzylphosphonate of m.p. 119°-121° C.

1. temperatureWith cooling
2. stirringstirring
3. customThe solvent is removed by distillation until the temperature
4. customis 115° C
5. washThe residual reaction solution is washed with 4×250 ml of water at 75° C.
6. customdried by azeotropic distillation
7. temperatureUpon cooling to room temperature
8. customthe product crystallises
9. filtrationis filtered with suction
10. washwashed with petroleum ether 100/140
11. customdried