HRID1672360

反应详情

EQUATION

反应方程式

HRID 1672360 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 6-chloro-N2-(pentan-3-yl)pyridine-2,3-diamine (936 mg, 4.37 mmol) in THF (10 mL) and CDI (1.1 g, 12.9 mmol) was added as a solid. After heating for 3 h, the reaction was cooled to room temperature. The excess CDI was quenched by the careful addition of water. The mixture was diluted with EtOAc and washed three times with water and once with brine. The solution was then dried over sodium sulfate, filtered and concentrated in vacuo. Silica gel chromatography (5%-40% EtOAc/hexanes) provided the title compound as a light purple solid (682 mg, 65%). m/z=240.0 (M+H)+

WORKUP

后处理

  1. temperatureAfter heating for 3 h
  2. customThe excess CDI was quenched by the careful addition of water
  3. additionThe mixture was diluted with EtOAc
  4. washwashed three times with water
  5. dry with materialThe solution was then dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo