HRID1294068

反应详情

EQUATION

反应方程式

HRID 1294068 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 5-bromo-2-nitropyridine-3-ylamine (436 mg, 2.0 mmol) in DMF (10 mL) was added Cs2CO3 (977 mg, 3.0 mmol) followed by 4-(t-butoxycarbonyl)aminophenol (459 mg, 2.2 mmol) in DMF (10 mL) at 0° C. then stirred at room temperature for 3 days. The mixture was extracted with ethyl acetate. The organic layer was washed with NaHCO3 (aq) and brine, dried over Na2SO4 then evaporated. Sequence purification on SiO2 column chromatography gave the title compound (624.2 mg, 90%): MS m/e 347 (M+1).

WORKUP

后处理

  1. extractionThe mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with NaHCO3 (aq) and brine
  3. dry with materialdried over Na2SO4
  4. customthen evaporated
  5. customSequence purification on SiO2 column chromatography