HRID2271393

反应详情

EQUATION

反应方程式

HRID 2271393 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Pd(PPh3)4 (23.1 mg, 0.02 mmol) and 3-((allyloxy)carbonyl)phenyl 3,4,5-tris(benzyloxy)benzoate (600 mg, 1 mmol) were dissolved in CH2Cl2 (3 mL) and cooled in an ice bath. To the resulting solution was added phenylsilane (216 mg, 2 mmol). After stirring for 15 min, H2O (5 mL) was added dropwise, resulting in a precipitate. The solid was washed successively with ethyl acetate, dichloromethane, and water. The combined organic layers were concentrated in vacuo to half-volume and extracted with water. The organic layer was dried over MgSO4, filtered, and concentrated in vacuo to provide the title compound (378 mg, 68%).

WORKUP

后处理

  1. temperaturecooled in an ice bath
  2. customresulting in a precipitate
  3. washThe solid was washed successively with ethyl acetate, dichloromethane, and water
  4. concentrationThe combined organic layers were concentrated in vacuo to half-volume
  5. extractionextracted with water
  6. dry with materialThe organic layer was dried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo