HRID861391

反应详情

EQUATION

反应方程式

HRID 861391 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-(4-trifluoromethyl-6-chloropyrimidin-5-yl)-1-(2-chloro-4-methoxypyrimidin-5-yl)methanol (0.21 g, 0.59 mmol) was stirred under a hydrogen atmosphere at room temperature with MgO (142 mg, 3.35 mmol, 6 equivalents), and 10% palladium on carbon (Pd/C) (25 mg, Degussa, 50% wet by weight). After 3 hours, an additional 30 mg of 10% Pd/C was added and the solution stirred for 4 hours, filtered over celite and concentrated in vacuo. Preparative radial chromatography (SiO2 ; hexane/EtOAc gradient elution) afforded the desired product, 81 mg (48%) as an oil.

WORKUP

后处理

  1. filtrationfiltered over celite and
  2. concentrationconcentrated in vacuo
  3. washPreparative radial chromatography (SiO2 ; hexane/EtOAc gradient elution)