HRID1843656

反应详情

EQUATION

反应方程式

HRID 1843656 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

300 mg (0.53 mmol) of 2,5-difluoro-N-(3-{1-(4-methoxybenzyl)-4-[2-(methylamino)-pyridin-4-yl]-1H-pyrazol-3-yl}phenyl)benzenesulfonamide were dissolved in 10 ml of trifluoroacetic acid and the mixture heated at 70° C. under stirring for 4 hours. The solvent was then removed in vacuo, the residue partitioned between dichloromethane and a saturated aqueous solution of sodium hydrogenocarbonate. The organic layer was dried over sodium sulphate and evaporated to dryness. The crude was finally purified by flash-chromatography on a silica gel column (CH2Cl2-CH3COCH3; from 9/1 to 8/2), giving 47 mg (20%) of the title compound.

WORKUP

后处理

  1. customThe solvent was then removed in vacuo
  2. customthe residue partitioned between dichloromethane
  3. dry with materialThe organic layer was dried over sodium sulphate
  4. customevaporated to dryness
  5. customThe crude was finally purified by flash-chromatography on a silica gel column (CH2Cl2-CH3COCH3; from 9/1 to 8/2)