HRID1958098

反应详情

EQUATION

反应方程式

HRID 1958098 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

To a solution of 3-bromo-2-cyclopropylmethoxy-5-nitro-pyridine (600 mg, 2.19 mmol) in methanol (30 ml) were added water (15 ml), zinc dust (1 g, 15.37 mmol) and ammonium chloride (1.28 g, 24.09 mmol) at 25° C., and the reaction mixture was stirred for 45 min at 25° C. After total consumption of starting material (monitored by TLC), the reaction mixture was filtered through a bed of celite, and the filtrate was evaporated under reduced pressure to get the crude residue. The residue was dissolved in dichloromethane and washed with water and brine. The organic part was dried over Na2SO4 and evaporated to get the compound (507 mg, 95%). This compound was used in next step without further purification. MS (LC/MS): 244.0 (M+H).

WORKUP

后处理

  1. customAfter total consumption of starting material (monitored by TLC)
  2. filtrationthe reaction mixture was filtered through a bed of celite
  3. customthe filtrate was evaporated under reduced pressure
  4. customto get the crude residue
  5. washwashed with water and brine
  6. dry with materialThe organic part was dried over Na2SO4
  7. customevaporated