HRID1986384

反应详情

EQUATION

反应方程式

HRID 1986384 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

Under nitrogen, to a solution of 2-bromo-5-nitro-4-pyridineamine (3.67 g, 16.8 mmol) and methyl 3-hydroxybenzoate (2.82 g, 18.5 mmol) in DMF (100 mL), was added NaH (810 mg, 60% suspension, 20.2 mmol). 5 min later, the reaction mixture was heated to 65° C. The reaction mixture was concentrated, taken up in EtOAC, washed with NaOH solution (1.0N), saturated NH4Cl solution and brine, dried over Na2SO4, filtered and concentrated to afford the title compound, which was used directly to next step without further purification. MS (ES+) m/e 290 [+H]+.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated
  2. washwashed with NaOH solution (1.0N), saturated NH4Cl solution and brine
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated