HRID1029261

反应详情

EQUATION

反应方程式

HRID 1029261 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 83 (135 mg, 0.59 mmol) in ether (10 mL) was added HCl (1.17 mL, 1.00 M, 1.17 mmol) in ether. The mixture was stirred for 3 h and the solvent was removed under vacuo. A suspension of this HCl salt in NMP (3 mL) was added N-(4-aminophenyl)-4-fluoro-2-(trifluoromethyl)benzamide (209 mg, 0.70 mmol). The mixture was stirred at 150° C. for 3 h. After cooling to room temperature, H2O was added. The resulting product precipitate and the solid was filtered, washed with H2O and MeOH, and dried under vacuum to provide 378 (210 mg, 73% yield) as pale solid.

WORKUP

后处理

  1. customthe solvent was removed under vacuo
  2. additionA suspension of this HCl salt in NMP (3 mL)
  3. stirringThe mixture was stirred at 150° C. for 3 h
  4. filtrationThe resulting product precipitate and the solid was filtered
  5. washwashed with H2O and MeOH
  6. customdried under vacuum