HRID1258721

反应详情

EQUATION

反应方程式

HRID 1258721 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-methylpropane-2-sulfinic acid chloride (83 mg, 0.59 mmol) in DCM (2 mL) was added dropwise to a solution of 4-chloro-3-[5-chloro-1-methyl-6-(4-trifluoromethyl-piperidin-1-yl)-1H-benzo[d]imidazol-2-ylamino]benzylamine (265 mg, 0.56 mmol), TEA (113 mg, 1.12 mmol) and DCM (3 mL) at 0° C. under Ar. The mixture was stirred at rt overnight, poured into H2O and extracted with DCM. The organic layer was washed with brine, dried over Na2SO4, filtered and concentrated. Crystallization from DCM/PE gave the sub-title compound.

WORKUP

后处理

  1. extractionextracted with DCM
  2. washThe organic layer was washed with brine
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customCrystallization from DCM/PE