HRID1360709

反应详情

EQUATION

反应方程式

HRID 1360709 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of 6-(2,4-difluorophenyl)-1-(2,6-difluorophenyl)-7-(hydroxymethyl)-2H-quinolizin-2-one (Example 50, 100 mg) was added Jones reagent (0.5 mL, 4 N in sulfuric acid; prepared using procedure similar to that disclosed in Bowers, Halsall, Jones, and Lemin, J. Chem. Soc., (1953), 2548-2560) at 0° C. The mixture was stirred for a couple of hours at 0° C. until reaction complete and then quenched with isopropanol (1 mL). After stirring for 10 min (green solution), the mixture was filtered through celite and concentrated. The residue was diluted with ethyl acetate and washed with water, brine, dried over MgSO4 and concentrated to give title compound (87 mg).

WORKUP

后处理

  1. customprepared
  2. customat 0° C
  3. customquenched with isopropanol (1 mL)
  4. stirringAfter stirring for 10 min (green solution)
  5. filtrationthe mixture was filtered through celite
  6. concentrationconcentrated
  7. additionThe residue was diluted with ethyl acetate
  8. washwashed with water, brine
  9. dry with materialdried over MgSO4
  10. concentrationconcentrated