HRID926460

反应详情

EQUATION

反应方程式

HRID 926460 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a 100 mL flask containing (4-chloro-2-methoxy-3-(4-(trifluoromethyl)benzyl)quinolin-6-yl)(2,6-dimethylpyridin-3-yl)methanol (1.51 g, 3.1 mmol, Intermediate 12: step e) was added 1,4-dioxane (50 mL) followed by activated MnO2 (1.3 g, 15 mmol) and the mixture was heated to reflux in an aluminum heating mantle under N2. After 1 hour, TLC (25% acetone:hexane) indicated that the reaction was complete. The contents were filtered while still hot through Celite® and rinsed with THF. The resulting light yellow solution was concentrated and chromatographed by passing through a silica gel column (10% acetone-hexane increasing to 25% acetone) to give the title compound as a light yellowish amorphous solid.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. filtrationThe contents were filtered while still hot through Celite®
  3. washrinsed with THF
  4. concentrationThe resulting light yellow solution was concentrated
  5. customchromatographed