HRID841

反应详情

EQUATION

反应方程式

HRID 841 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2-[(3,5-Dimethylphenyl)thio]-6-fluorobenzonitrile (Example 18) (1.0 g, 3.9 mmol) was dissolved in 100 ml of methanol. A solution of OXONE®.dagger. (2.63 g, 4.3 mmol) in 15 ml of water was added dropwise with stirring. After stirring 1.5 h, the solid was removed by vacuum filtration and washed with 3×50 ml of methanol. The filtrate was concentrated to dryness and chromatographed on silica get (flash; Hex/EtOAc 2:1) to provide 0.5 g (47%) of 2-[(3,5-dimethylphenyl)sulfinyl]-6-fluorobenzonitrile: mp 146°-147° C.

WORKUP

后处理

  1. stirringAfter stirring 1.5 h
  2. customthe solid was removed by vacuum filtration
  3. washwashed with 3×50 ml of methanol
  4. concentrationThe filtrate was concentrated to dryness
  5. customchromatographed on silica
  6. customget (flash; Hex/EtOAc 2:1)