HRID1672359

反应详情

EQUATION

反应方程式

HRID 1672359 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a room-temperature solution containing 6-chloro-3-nitro-N-(pentan-3-yl)pyridin-2-amine (1.8 g, 7.4 mmol) in MeOH (10 mL) and EtOAc (10 mL) was added SnCl2 dihydrate (10.0 g, 44.3 mmol). After 3 h, the reaction mixture was concentrated in vacuo and then re-dissolved in EtOAc and water. After stirring overnight, the layers were separated and the organic layer was dried over sodium sulfate, filtered, and concentrated in vacuo. Silica gel chromatography (25%-50% EtOAc/Hexanes) provided the title compound as a white solid (940 mg, 57%). m/z=223.2 (M+H)+

WORKUP

后处理

  1. concentrationthe reaction mixture was concentrated in vacuo
  2. dissolutionre-dissolved in EtOAc
  3. customthe layers were separated
  4. dry with materialthe organic layer was dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo