HRID2041569

反应详情

EQUATION

反应方程式

HRID 2041569 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

Add manganese dioxide (1.44 g) to a stirred solution of [4-(tert-butyldimethylsilyloxymethyl)-phenyl]-pyridin-3-yl-methanol (360 mg, 0.303 mmol) in anhydrous 1,4-dioxane (25 mL). Heat the mixture to 70° C. overnight. Cool the reaction mixture to room temperature, filter through Celite® and wash with EtOAc. Concentrate the filtrate in vacuo. Purify the crude mixture by chromatography on silica gel eluting sequentially with hexane and hexane/EtOAc (1:1) to provide the desired intermediate (233 mg, 65%). GC-MS m/z: 327 (M+).

WORKUP

后处理

  1. temperatureCool the reaction mixture to room temperature
  2. filtrationfilter through Celite®
  3. washwash with EtOAc
  4. concentrationConcentrate the filtrate in vacuo
  5. customPurify the crude mixture by chromatography on silica gel eluting sequentially with hexane and hexane/EtOAc (1:1)