HRID627506

反应详情

EQUATION

反应方程式

HRID 627506 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

1,4-dioxane (7.5 mL) and manganese (IV) dioxide (447 mg, 5.14 mmol) were added to crude (2,4-dichloro-3-phenylquinolin-6-yl)(3-methylisoxazol-5-yl)methanol (Intermediate 37, step a, 1.03 mmol assuming theoretical yield in prior step). The resulting black suspension was heated in a 100° C. oil bath in a sealed tube for 3 hours. The mixture was allowed to cool, was diluted with DCM, and was filtered through Celite®. The filtrate was concentrated and the residue was purified by flash column chromatography (silica gel, 3-15% EtOAc-heptane) to afford slightly impure title compound which was used without further purification.

WORKUP

后处理

  1. customassuming theoretical yield in prior step)
  2. temperatureto cool
  3. filtrationwas filtered through Celite®
  4. concentrationThe filtrate was concentrated
  5. customthe residue was purified by flash column chromatography (silica gel, 3-15% EtOAc-heptane)