HRID517929

反应详情

EQUATION

反应方程式

HRID 517929 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 2-bromo-3-chloro-7,8-dihydro-5H-pyrido[2,3-b]pyrazin-6-one (prepared according to the preparation procedures disclosed in PCT patent application PCT/EP2011/062028, Intermediate J) (3.9 g, 14.86 mmol) and ethyl 7-bromoheptanoate (7.05 g, 29.7 mmol) in DMF (75 ml) under a nitrogen atmosphere was treated with potassium carbonate (10.27 g, 74.3 mmol) and the resulting solution was stirred at room temperature for 4 days. The mixture was diluted with water and extracted with EtOAc (×2). The extracts were washed with water and brine, dried (MgSO4) and evaporated under vacuum. The crude product was purified by chromatography on silica eluting with 0-60% EtOAc in iso-hexane to afford the titled compound;

WORKUP

后处理

  1. customaccording to the preparation procedures
  2. extractionextracted with EtOAc (×2)
  3. washThe extracts were washed with water and brine
  4. dry with materialdried (MgSO4)
  5. customevaporated under vacuum
  6. customThe crude product was purified by chromatography on silica eluting with 0-60% EtOAc in iso-hexane