HRID1931081

反应详情

EQUATION

反应方程式

HRID 1931081 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of Example 32B (2 g, 8.92 mmol), 1H-benzo[d][1,2,3]triazol-1-ol hydrate (1.37 g, 8.92 mmol), N1-((ethylimino)methylene)-N3,N3-dimethylpropane-1,3-diamine hydrochloride (1.71 g, 8.92 mmol), 2-fluoro-5-(trifluoromethyl)benzoic acid (1.86 g, 8.92 mmol), and triethylamine (1.86 mL, 13.37 mmol) in 30 mL of THF was heated at 80° C. for 12 hr. The mixture was cooled to room temperature, diluted with EtOAc, washed with NaHCO3, dried over MgSO4 and concentrated. The residue was purified by flash chromatography on SiO2 (Hexanes: EtOAc, 0 to 50%) to give the title compound. MS (ESI) m/z 415 (M+H)+.

WORKUP

后处理

  1. washwashed with NaHCO3
  2. dry with materialdried over MgSO4
  3. concentrationconcentrated
  4. customThe residue was purified by flash chromatography on SiO2 (Hexanes: EtOAc, 0 to 50%)