反应 #806259

反应方程式

2,2,4-trimethylpentan-1,3-diol

NaOH

methallyl chloride

→

1-(2-methyl-2-propenyloxy)-2,2,4-trimethylpentan-3-ol

收率 101.8%

反应条件

后处理

1. 1
   其他To a 1 L flask equipped with a reflux condenser
2. 2
   温度This mixture was heated in an oil bath
3. 3
   其他reached 50° C.
4. 4
   workup.ADDITIONDuring the addition
5. 5
   温度The reaction mixture was cooled
6. 6
   其他quenched with 400 ml of water
7. 7
   萃取extracted twice with 100 ml of toluene
8. 8
   洗涤The combined organic layers were washed with 50 ml of saturated ammonium chloride and 50 ml of saturated sodium chloride
9. 9
   其他evaporated

实验过程

To a 1 L flask equipped with a reflux condenser and a thermometer, was added 292.5 g (2.0 mol) of 2,2,4-trimethylpentan-1,3-diol, 352.0 g (4.4 mol) of 50% aqueous NaOH, and 6.45 g (20 mmol) of tetrabutyl ammonium bromide. This mixture was heated in an oil bath and when the reaction mixture reached 50° C., 199.2 g (2.2 mol) of methallyl chloride was added drop-wise over 50 minutes. During the addition, the oil bath temperature was gradually raised to 100° C. and the reaction was continued for an additional 3 hours at 100° C. The reaction mixture was cooled, quenched with 400 ml of water, and extracted twice with 100 ml of toluene. The combined organic layers were washed with 50 ml of saturated ammonium chloride and 50 ml of saturated sodium chloride and evaporated to give 408 g of crude 1-(2-methyl-2-propenyloxy)-2,2,4-trimethylpentan-3-ol. After reduced pressure distillation (71–80° C., 3 mmHg), 377.1 g (yield 94.1%) of 1-(2-methyl-2-propenyloxy)-2,2,4-trimethylpentan-3-ol was obtained.

来源