HRID80413

反应详情

EQUATION

反应方程式

HRID 80413 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

To a flame dried, 500 mL round bottomed flask equipped with an addition funnel charged with epichlorohydrin (15.62 g, 0.17 moles), is added 2-ethylhexanol (16.5 g, 0.127 moles) and stannic chloride (0.20 g, 0.001 moles). The reaction is kept under an argon atmosphere and warmed to 90° C. using an oil bath. Epichlorohydrin is dripped into the stirring solution over 60 minutes followed by stirring at 90° C. for 18 hours. The reaction is fitted with a vacuum distillation head and 1-chloro-3-(2-ethyl-hexyloxy)-propan-2-ol is distilled under 0.2 mm Hg. The 1-chloro-3-(2-ethyl-hexyloxy)-propan-2-ol (4.46 g, 0.020 moles) is dissolved in tetrahydrofuran (50 mL) and stirred at room temperature under an argon atmosphere. To the stirring solution is added potassium tert-butoxide (2.52 g, 0.022 moles) and the suspension is stirred at room temperature for 18 hours. The reaction is then evaporated to dryness, residue dissolved in hexanes and washed with water (100 mL). The hexanes phase is separated, dried with Na2SO4, filtered and evaporated to dryness to yield the crude 2-ethylhexyl glycidyl ether, which can be further purified by vacuum distillation.

WORKUP

后处理

  1. customTo a flame dried
  2. custom500 mL round bottomed flask equipped with an addition funnel
  3. distillationis distilled under 0.2 mm Hg
  4. stirringstirred at room temperature under an argon atmosphere
  5. stirringthe suspension is stirred at room temperature for 18 hours
  6. customThe reaction is then evaporated to dryness, residue
  7. dissolutiondissolved in hexanes
  8. washwashed with water (100 mL)
  9. customThe hexanes phase is separated
  10. dry with materialdried with Na2SO4
  11. filtrationfiltered
  12. customevaporated to dryness