HRID400233

反应详情

EQUATION

反应方程式

HRID 400233 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-40 °C

PROCEDURE

实验过程

A solution of 4-benzyloxy-2,3-epoxy-1-butanol (6.28 g, 32.37 mmol) in anhydrous tetrahydrofuran (75 mL) was added dropwise at -40° C. over a period of 45 minutes, to a 2M solution of allyl magnesium chloride (48.5 mL, 97 mmol) and tetrahydrofuran (50 mL). The solution was stirred at -40° C. for 1 hour, warmed to 0° C. and quenched by addition of aqueous ammonium chloride solution. The tetrahydrofuran layer was separated and the aqueous layer was extracted with ethyl acetate (three times). The combined organic extract was dried (magnesium sulfate), filtered and concentrated to obtain a mixture of compounds A and B.

WORKUP

后处理

  1. temperaturewarmed to 0° C.
  2. customquenched by addition of aqueous ammonium chloride solution
  3. customThe tetrahydrofuran layer was separated
  4. extractionthe aqueous layer was extracted with ethyl acetate (three times)
  5. extractionThe combined organic extract
  6. dry with materialwas dried (magnesium sulfate)
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customto obtain