HRID64175

反应详情

EQUATION

反应方程式

HRID 64175 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of N-(3-(3-fluoropyridin-2-yl)-5-nitrophenyl)acetamide (5 g, 18.18 mmol) in THF (50 ml), Zn (11.8 g, 181.18 mmol) was added followed by slow addition of solution of NH4Cl (9.7 g, 181.18 mmol) in 20 ml water. The mixture was stirred at RT for 1 h. The mixture was filtered through celite and bed washed with ethyl acetate. The mixture was diluted with ethyl acetate and washed with water and brine solution, dried over sodium sulphate and distilled to give the product in 90% yield (4.2 g). LC-MS (ESI): Calculated mass: 245; Observed mass: 246.1 [M+H]+ (rt: 0.21 min).

WORKUP

后处理

  1. filtrationThe mixture was filtered through celite and bed
  2. washwashed with ethyl acetate
  3. additionThe mixture was diluted with ethyl acetate
  4. washwashed with water and brine solution
  5. dry with materialdried over sodium sulphate
  6. distillationdistilled
  7. customto give the product in 90% yield (4.2 g)
  8. custom246.1 [M+H]+ (rt: 0.21 min)