HRID1672357

反应详情

EQUATION

反应方程式

HRID 1672357 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a room-temperature mixture containing 6-chloro-3-nitro-N-(pentan-3-yl)pyridin-2-amine (250 mg, 0.90 mmol) and potassium carbonate (250 mg, 1.8 mmol) in acetonitrile (2 mL) was added dimethylamine (1.35 mL, 1.0 M, 1.35 mmol) by syringe. After 3 h, the reaction mixture was concentrated in vacuo and then re-dissolved in EtOAc and water. The organic layer was washed twice with water and once with brine, dried over sodium sulfate, filtered and concentrated In vacuo. Silica gel chromatography (5%-20% EtOAc/Hexanes) provided the title compound as a yellow solid (119 mg, 52%). m/z=253.2 (M+H)+

WORKUP

后处理

  1. concentrationthe reaction mixture was concentrated in vacuo
  2. dissolutionre-dissolved in EtOAc
  3. washThe organic layer was washed twice with water and once with brine
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated In vacuo