HRID657102

反应详情

EQUATION

反应方程式

HRID 657102 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of N2-[2,2-bis(methyloxy)ethyl]-6-(methyloxy)-2,3-pyridinediamine (2.2 g, 10 mmol), ethyl bromoacetate (1.1 mL, 1.65 g, 10 mmol) and potassium carbonate (2.1 g, 20 mmol) in acetonitrile (50 mL) and DMF (5 mL) was stirred at room temperature overnight. The mixture was filtered and evaporated. The residue was dissolved in ethyl acetate and washed with water and brine. The organic extract was concentrated and added to a silica column which was then eluted with 0-100% ethyl acetate in hexane affording product (2.5 g, 82%).

WORKUP

后处理

  1. filtrationThe mixture was filtered
  2. customevaporated
  3. dissolutionThe residue was dissolved in ethyl acetate
  4. washwashed with water and brine
  5. extractionThe organic extract
  6. concentrationwas concentrated
  7. additionadded to a silica column which
  8. washwas then eluted with 0-100% ethyl acetate in hexane affording product (2.5 g, 82%)