HRID2189775

反应详情

EQUATION

反应方程式

HRID 2189775 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-Cyano-4-[(1-methylethyl)oxy]benzoyl chloride (D106) (545 mg, 2.437 mmol) and N-hydroxy-1H-indazole-5-carboximidamide (D2) (685 mg, 2.437 mmol) were dissolved in acetonitrile (30 ml) before adding triethylamine (0.374 ml, 2.68 mmol). The resulting mixture was stirred at room temperature for 3 h then at 80° C. for 48 h, then cooled at room temperature. The precipitate formed was filtered off and dissolved in EtOAc and washed with water, evaporated and chromatographed [0-15% EtOAc in cyclohexane] to give the title compound (170 mg, 17%) as a pink solid. MS (ES): C19H15N5O2 requires 345; found (MH+) 346

WORKUP

后处理

  1. waitat 80° C. for 48 h
  2. temperaturecooled at room temperature
  3. customThe precipitate formed
  4. filtrationwas filtered off
  5. dissolutiondissolved in EtOAc
  6. washwashed with water
  7. customevaporated
  8. customchromatographed [0-15% EtOAc in cyclohexane]