HRID2189736

反应详情

EQUATION

反应方程式

HRID 2189736 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A solution of Ethyl 3-{5-[(hydroxyamino)(imino)methyl]-1H-indazol-1-yl}propanoate (D52) (2.04 g, 7.38 mmol), 3-chloro-4-[(1-methylethyl)oxy]benzoic acid (D3) (1.743 g, 8.12 mmol), EDC (2.123 g, 11.08 mmol) and HOBT (1.357 g, 8.86 mmol) in N,N-Dimethylformamide (DMF) (25 ml) was stirred overnight then heated at 120° C. during 4 hours. The mixture was dissolved in EtOAc then washed with water and NaHCO3 and purified by flash chromatography, eluting with EtOAc/iso-Hexane 10-90% then 10-30%. The solvent was evaporated to give (1.95 g) of white solid. MS (ES): C23H2335ClN4O4 requires 454; found (MH+) 455.

WORKUP

后处理

  1. washthen washed with water and NaHCO3
  2. custompurified by flash chromatography
  3. washeluting with EtOAc/iso-Hexane 10-90%
  4. customThe solvent was evaporated