HRID2276571

反应详情

EQUATION

反应方程式

HRID 2276571 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

A mixture of ethyl 7-(2-bromo-3-chloro-7,8-dihydropyrido[2,3-b]pyrazin-5(6H)-yl)heptanoate (step 2) (100 mg, 0.247 mmol) and potassium carbonate (102 mg, 0.741 mmol) in dioxane (2 ml) was degassed by bubbling nitrogen through (×3). Pd(Ph3P)4 (28.6 mg, 0.025 mmol) was added and the mixture was degassed by bubbling nitrogen through (×3). The mixture was heated at 150° C. for 2 hours using microwave irradiation. The mixture was diluted with water and extracted with EtOAc (×2). The organics were washed with brine, dried (MgSO4) and evaporated under vacuum to a pale oil. The crude was purified by chromatography on silica eluting with 20-100% EtOAc/iso-hexane to give the title compound as a clear oil;

WORKUP

后处理

  1. customwas degassed
  2. customby bubbling nitrogen through (×3)
  3. customthe mixture was degassed
  4. customby bubbling nitrogen through (×3)
  5. custommicrowave irradiation
  6. additionThe mixture was diluted with water
  7. extractionextracted with EtOAc (×2)
  8. washThe organics were washed with brine
  9. dry with materialdried (MgSO4)
  10. customevaporated under vacuum to a pale oil
  11. customThe crude was purified by chromatography on silica eluting with 20-100% EtOAc/iso-hexane