HRID2211272

反应详情

EQUATION

反应方程式

HRID 2211272 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of 23.2 g (0.2 mol) of 3-ethyl-3-hydroxymethyloxetane in 48.4 g (0.4 mol) of allylbromide and 50 g of a 50 wt % aqueous solution of potassium hydroxide in a 300 mL round bottom flask equipped with a magnetic stirrer was added 1.0 g of tetra-n-butylammonium bromide with vigorous stirring at 0° C. After 24 hrs, 100 mL of dichlorometane and 100 mL of water were added to the reaction mixture. The organic phase was washed with water twice, dried over magnesium sulfate, filtered and the solvent removed on a rotary evaporator. The residue was purified by distillation under vacuum, giving 28.6 g of 3-ethyl-3-allyloxymethyloxetane (yield 92%, b.p.:55° C. at 1.5 mm Hg).

WORKUP

后处理

  1. washThe organic phase was washed with water twice
  2. dry with materialdried over magnesium sulfate
  3. filtrationfiltered
  4. customthe solvent removed on a rotary evaporator
  5. distillationThe residue was purified by distillation under vacuum