HRID1258731

反应详情

EQUATION

反应方程式

HRID 1258731 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of N-(4-trifluoromethyl-3-(5-chloro-1-methyl-6-(4-trifluoromethyl-piperidin-1-yl)-1H-benzo[d]imidazol-2-ylamino)benzyl)-2-methylpropane-2-sulfinamide (140 mg, 0.23 mmol), m-chloroperoxybenzoic acid (198 mg, 1.15 mmol) and CHCl3 (7 mL) was stirred at rt for 15 min. The mixture was poured into brine and extracted with DCM. The organic layer was dried over Na2SO4, filtered and concentrated. The residue was mixed with PBr3 (144 mg, 0.50 mmol) and DCM (5 ml) and the mixture was stirred at rt overnight. The mixture was poured into H2O and extracted with DCM. The organic layer was washed with brine, dried over Na2SO4, filtered and concentrated. Purification by column chromatography gave the title compound.

WORKUP

后处理

  1. extractionextracted with DCM
  2. dry with materialThe organic layer was dried over Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated
  5. stirringthe mixture was stirred at rt overnight
  6. extractionextracted with DCM
  7. washThe organic layer was washed with brine
  8. dry with materialdried over Na2SO4
  9. filtrationfiltered
  10. concentrationconcentrated
  11. customPurification by column chromatography