HRID481523

反应详情

EQUATION

反应方程式

HRID 481523 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of Compound 45 (3.0 g, 17 mmol) and CBr4 (11 g, 34 mmol) in CH2Cl2 (100 ml) was added PPh3 (18 g, 67 mmol) at r.t., and stirred for 1.5 h. The mixture was quenched by the addition of H2O, and extracted with CH2Cl2. The combined organic layers were washed with brine, dried over MgSO4, filtered, and concentrated. This was purified by SiO2 chromatography to give Compound 53 (2.5 g, 45%) as a colorless oil.

WORKUP

后处理

  1. customThe mixture was quenched by the addition of H2O
  2. extractionextracted with CH2Cl2
  3. washThe combined organic layers were washed with brine
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThis was purified by SiO2 chromatography