HRID1269855

反应详情

EQUATION

反应方程式

HRID 1269855 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The 2-(1H-indazol-5-yloxy)benzoic acid (80.8 mg, 0.318 mmol) synthesized in Example 479 and dimethylamine hydrochloride (33.7 mg, 0.413 mmol) were dissolved in N,N-dimethylformamide (2 ml), and 1-ethyl-3-(3′-dimethylaminopropyl)carbodiimide monohydrochloride (72.5 mg, 0.380 mmol), hydroxybenzotriazole (47.1 mg, 0.349 mmol) and triethylamine (0.13 ml, 0.954 mmol) were added thereto at room temperature and then stirred for 2.5 hours. After the reaction, a saturated aqueous sodium hydrogencarbonate solution was added thereto, followed by extraction with chloroform. The organic layer was washed with a saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate, and then concentrated to obtain 2-(1H-indazol-5-yloxy)-N,N-dimethylbenzamide (51 mg, 57%).

WORKUP

后处理

  1. customAfter the reaction
  2. extractionfollowed by extraction with chloroform
  3. washThe organic layer was washed with a saturated aqueous sodium chloride solution
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated