HRID1829591

反应详情

EQUATION

反应方程式

HRID 1829591 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

BF3—OEt2 (2.0 ml) is added dropwise to a solution of 1-cyclohexylethanol (16.6 g, 127.0 mmol) and isobutylene oxide (2.9 g, 40.0 mmol) in cyclohexane (20 ml) that has been cooled to 0° C. The reaction mixture is now stirred at 0° C. for a further 30 minutes, and further, BF3—OEt2 (2.0 ml) is then added. After a further 3 hours at 0° C., the cooling is removed and the reaction solution is washed once with 1 M NaOH (15 ml). The organic phase is dried over Na2SO4, filtered off and freed from solvent in a rotary evaporator. The 1-cyclohexylethanol that has not completely reacted is removed from the crude product; thus, obtained by means of bulb tube distillation (BTD) and 5.3 g crude 2-(1-cyclohexylethoxy)-2-methyl-1-propanol is obtained which has a GC content of 75% and can be used in the next reaction without further purification.

WORKUP

后处理

  1. waitAfter a further 3 hours at 0° C.
  2. customthe cooling is removed
  3. washthe reaction solution is washed once with 1 M NaOH (15 ml)
  4. dry with materialThe organic phase is dried over Na2SO4
  5. filtrationfiltered off
  6. customfreed from solvent in a rotary evaporator
  7. customThe 1-cyclohexylethanol that has not completely reacted
  8. customis removed from the crude product
  9. customthus, obtained by means of bulb tube
  10. distillationdistillation (BTD)