HRID427502

反应详情

EQUATION

反应方程式

HRID 427502 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Ethyl 5,6-diaminonicotinate (1.4 g, 7.7 mmol) and 3-bromo-2-butanon (1.16 g, 7.2 mmol) were added to 1,2-dimethoxyethan (50 ml) and refluxed for 20 h. The solvent was evaporated under reduced pressure and the residue was dissolved in methylene chloride. The methylene chloride solution was washed with saturated sodium bicarbonate and dried (Na2SO4). The solvent was evaporated under reduced pressure and the residue was purified by column chromatography on silica gel using methylene chloride:methanol (10:1) as eluent to give 0.3 g (17%) of the title compound.

WORKUP

后处理

  1. temperaturerefluxed for 20 h
  2. customThe solvent was evaporated under reduced pressure
  3. dissolutionthe residue was dissolved in methylene chloride
  4. washThe methylene chloride solution was washed with saturated sodium bicarbonate
  5. dry with materialdried (Na2SO4)
  6. customThe solvent was evaporated under reduced pressure
  7. customthe residue was purified by column chromatography on silica gel