HRID1428963

反应详情

EQUATION

反应方程式

HRID 1428963 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

N-Cyclopropyl-N-{1-[2-(2-oxo-oxazolidin-3-yl)-benzoyl]-piperidin-4-yl}-3-trifluoromethyl-benzenesulfonamide (12) (0.110 g, 0.20 mmol) was taken up in 3 ml of ETOH and 0.5 ml of water. To the mixture, KOH (0.046 g, 0.82 mmol) was added. The mixture was heated at 100° C. and stirred for 2 hours. The reaction mixture was concentrated to dryness under reduced pressure. Then residue was dissolved in EtOAc (30 ml) and the mixture was washed with H2O (15 ml) and brine (15 ml). The organic layer was dried over MgSO4 and concentrated to dryness. The crude product was purified through a column of silica gel with a gradient of 90% to 100% EtOAc in hexane to afford the title compound 13 (pale yellow solid, 81 mg, 83%). LC: 100%. MS: m/z=511.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated to dryness under reduced pressure
  2. dissolutionThen residue was dissolved in EtOAc (30 ml)
  3. washthe mixture was washed with H2O (15 ml) and brine (15 ml)
  4. dry with materialThe organic layer was dried over MgSO4
  5. concentrationconcentrated to dryness
  6. customThe crude product was purified through a column of silica gel with a gradient of 90% to 100% EtOAc in hexane