反应详情

温度

111 °C

A 1 liter, 4-neck round-bottom flask fitted with mechanical stirrer, pressure equalizing addition funnel (nitrogen inlet), thermocouple connected to a controller and mantle for heating, a 5-plate Oldershaw column and vacuum type distilling head with finger type condenser and stopcock to control the reflux ratio was charged with 201 g (1.50 mol) trimethylolpropane, 100 g (0.63 mol) tert.-butyl acetoacetate and 282 g of toluene. An additional 626.5 g (3.96 mol) of tert.-butyl acetoacetate was charged to the addition funnel. A slow nitrogen flow was maintained through the addition funnel and reactor and the mixture was heated to about 111° C. Reflux began when the flask contents reached about 111° C. and the reflux ratio/take-off was adjusted to keep the head temperature between 82-84° C. The additional tert.-butyl acetoacetate was gradually added over about 4 hr as 442 ml of distillate was collected. The pot temperature increased gradually to 117° C. during the addition. Distillation continued: the pot temperature gradually increased to 132° C. and the head temperature increased to 109° C. over an additional 2.3 hr. Total distillate collected was 472 g determined to be 70.59% tert.-butanol or 100.1% of theory.

1. customA 1 liter, 4-neck round-bottom flask fitted with mechanical stirrer
2. additionaddition funnel (nitrogen inlet)
3. temperaturemantle for heating
4. distillationa 5-plate Oldershaw column and vacuum type distilling head with finger type condenser
5. temperatureA slow nitrogen flow was maintained through the addition funnel and reactor
6. temperatureReflux
7. customreached about 111° C.
8. temperaturethe reflux ratio/take-off
9. custombetween 82-84° C
10. customwas collected
11. temperatureThe pot temperature increased gradually to 117° C. during the addition
12. distillationDistillation
13. temperaturethe pot temperature gradually increased to 132° C.
14. temperaturethe head temperature increased to 109° C. over an additional 2.3 hr
15. distillationTotal distillate collected