HRID541954

反应详情

EQUATION

反应方程式

HRID 541954 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A solution of 4-(2-bromo-4-nitrophenyl)morpholine (0.27 g, 0.95 mmol), tert-butyl (3-ethynylphenyl)carbamate, and bis(triphenylphosphine)palladium(II) chloride (67 mg, 95 μmol) in N,N-dimethylformamide (4.4 mL) was treated with N,N-diisopropylethylamine (0.21 mL, 1.2 mmol) and stirred at 80° C. for 16 h. The reaction mixture was diluted with ethyl acetate, washed with brine, dried over anhydrous sodium sulfate, filtered, and evaporated to give a crude residue. This material was purified by flash column chromatography to give the desired product (0.28 g, 70%) as a solid. LCMS for C23H26N3O5 (M+H)+: m/z=424.0.

WORKUP

后处理

  1. washwashed with brine
  2. dry with materialdried over anhydrous sodium sulfate
  3. filtrationfiltered
  4. customevaporated
  5. customto give a crude residue
  6. customThis material was purified by flash column chromatography