HRID2190537

反应详情

EQUATION

反应方程式

HRID 2190537 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 3-tert-butyl-phenylamine was added 4-bromo-3-fluoro-benzoic acid, DMF (21 mL) and EDCI and were stirred at room temperature overnight. The reaction was diluted with DCM (8 mL) and was washed with HCl (1 M, 8 mL), NaOH (1 M, 8 mL), and brine (5 mL), dried over Na2SO4, and concentrated by stream of nitrogen. The resulting viscous oil was purified by flash chromatography with increasing concentration ethyl acetate in hexanes to afford the product. LCMS calcd for C17H17FNO (m/e) 349, obsd 350 (M+H).

WORKUP

后处理

  1. washwas washed with HCl (1 M, 8 mL), NaOH (1 M, 8 mL), and brine (5 mL)
  2. dry with materialdried over Na2SO4
  3. concentrationconcentrated by stream of nitrogen
  4. customThe resulting viscous oil was purified by flash chromatography
  5. temperaturewith increasing
  6. concentrationconcentration ethyl acetate in hexanes
  7. customto afford the product