HRID423182

反应详情

EQUATION

反应方程式

HRID 423182 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

3-Bromo-pyridine-2-carboxylic acid methyl ester (12.8 g, 59.2 mmol) is dissolved in methanol (150 mL) and cooled to 0° C. To the mixture is added NaBH4 (11.2 g, 296 mmol) in 1.0 g portions. The mixture is warmed to room temperature and stirred for 3 h. The methanol is removed under reduced pressure, AcOEt is added and the solution is washed with saturated, aqueous ammonium chloride and brine. The organic portion is dried over MgSO4, filtered, and concentrated under reduced pressure to yield 6.8 g (62%) of the title compound as a white solid. GCMS m/e 187 [M−H]−.

WORKUP

后处理

  1. temperatureThe mixture is warmed to room temperature
  2. customThe methanol is removed under reduced pressure, AcOEt
  3. additionis added
  4. washthe solution is washed with saturated, aqueous ammonium chloride and brine
  5. dry with materialThe organic portion is dried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure