反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customwas degassed
- customby bubbling nitrogen through (×3)
- customthe mixture was degassed
- customby bubbling nitrogen through (×3)
- custommicrowave irradiation
- additionThe mixture was diluted with water
- extractionextracted with EtOAc (×2)
- washThe organics were washed with brine
- dry with materialdried (MgSO4)
- customevaporated under vacuum to a pale oil
- customThe crude was purified by chromatography on silica eluting with 20-100% EtOAc/iso-hexane