HRID2390773

反应详情

EQUATION

反应方程式

HRID 2390773 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

m-Chloroperbenzoic acid (4.71 g, 27.3 mmol) and anhydrous magnesium sulfate (6.57 g, 54.6 mmol) in dichloromethane (100 mL) were dissolved at room temperature for 1 hour with stirring. To this solution was added [3-(3-methoxy-5-methylphenyl)-4-(2-methylthio-pyrimidin-4-yl)pyrazol-1-yl]acetonitrile (1.6 g, 4.55 mmol) which was subjected to oxidation to sulfone by stirring for an additional two hours. After completion of the reaction, the precipitate was filtered off and washed with dichloromethane. The filtrate was washed with brine and dichloromethane, and the organic layer was separated, dried over anhydrous magnesium sulfate and concentrated through vacuum distillation. The residue was purified by column chromatography to give the title compound (1.23 g, 70.4%).

WORKUP

后处理

  1. stirringby stirring for an additional two hours
  2. customAfter completion of the reaction
  3. filtrationthe precipitate was filtered off
  4. washwashed with dichloromethane
  5. washThe filtrate was washed with brine and dichloromethane
  6. customthe organic layer was separated
  7. dry with materialdried over anhydrous magnesium sulfate
  8. concentrationconcentrated through vacuum distillation
  9. customThe residue was purified by column chromatography