HRID735460

反应详情

EQUATION

反应方程式

HRID 735460 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

Next, a solution of (6-fluoro-5-trifluoromethyl-cyclohexa-2,4-dienyl)-pyridin-2-yl-methanone (1.5 g, 5.6 mmol), 4-dimethylaminopyridine (0.5 g) and hydrazine hydrate (5 mL) in pyridine (20 mL) was heated at 100° C. overnight. The reaction mixture was cooled and diluted with brine and EtOAc. The organics were washed with water (3×25 mL), then brine (25 mL) and dried over MgSO4. The reaction mixture was concentrated in vacuo and purified by flash chromatography (silica gel 60, EtOAc/CH2Cl2, 19:1) to afford 3-pyridin-2-yl-7-(trifluoromethyl)-2H-indazole as a pale yellow solid (1.1 g, 76%).

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled
  2. washThe organics were washed with water (3×25 mL)
  3. dry with materialbrine (25 mL) and dried over MgSO4
  4. concentrationThe reaction mixture was concentrated in vacuo
  5. custompurified by flash chromatography (silica gel 60, EtOAc/CH2Cl2, 19:1)