HRID2189775
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- waitat 80° C. for 48 h
- temperaturecooled at room temperature
- customThe precipitate formed
- filtrationwas filtered off
- dissolutiondissolved in EtOAc
- washwashed with water
- customevaporated
- customchromatographed [0-15% EtOAc in cyclohexane]