HRID59654

反应详情

EQUATION

反应方程式

HRID 59654 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-{Amino-[6-oxo-2-(3-trifluoromethyl-phenylamino)-cyclohex-1-enyl]-methyl}-3-bromo-benzonitrile (INTERMEDIATE 21, 16.5 g, 33 mmol) is suspended in acetonitrile (150 mL) and triethylamine (3.47 mL, 24.7 mmol) and 1,1′-carbonyldiimidazole (6.7 g, 41.2 mmol) are added. The mixture is stirred at room temperature for 1 h. The solvent is evaporated under reduced pressure and water is added. The product precipitates; the precipitate is filtered off, washed with water and dried. Yield: 14 g. ESI mass spectrum: [M+H]+=490 (bromine isotope pattern); Retention time HPLC: 0.64 min (X012_S02).

WORKUP

后处理

  1. customThe solvent is evaporated under reduced pressure and water
  2. additionis added
  3. customThe product precipitates
  4. filtrationthe precipitate is filtered off
  5. washwashed with water
  6. customdried
  7. custom0.64 min (X012_S02)