HRID2105024

反应详情

EQUATION

反应方程式

HRID 2105024 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 4-(2-bromophenyl)-1H-imidazole (880 mg, 3.94 mmol) in 10 mL DMF, were added TEA (0.605 mL, 4.34 mmol) and trityl chloride (1.21 g, 4.34 mmol). The mixture was stirred at rt for 14 h, then diluted with EtOAc. The organic phase was washed with H2O (2×) and brine, dried (Na2SO4), filtered through a 1″ pad of silica gel and concentrated. The crude product was purified by flash chromatography (0 to 40% EtOAc/hexanes gradient) to afford 1.34 g of Intermediate 217.1 as an off-white solid. LCMS (50 to 100% B, 4 min gradient, A 95% H2O/5% CH3CN/0.1% TFA, B=5% H2O/95% CH3CN/0.1% TFA) RT=0.77 min, 465.2 (M+H)+.

WORKUP

后处理

  1. washThe organic phase was washed with H2O (2×) and brine
  2. dry with materialdried (Na2SO4)
  3. filtrationfiltered through a 1″ pad of silica gel
  4. concentrationconcentrated
  5. customThe crude product was purified by flash chromatography (0 to 40% EtOAc/hexanes gradient)