HRID710269
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
- 155 °C
PROCEDURE
实验过程
(S)-tert-Butyl 2-(4-(3-chloropyridin-2-ylamino)phenyl)morpholine-4-carboxylate (47 mg, 0.12 mmol), palladium(II)-acetate (2.7 mg, 0.012 mmol), tricyclohexylphosphine tetrafluoroborate (9 mg, 0.024 mmol) and DBU (37 mg, 0.24 mmol) were dissolved in a mixture of o-xylene (0.7 ml) and dimethylacetamide (0.7 ml). The mixture was degassed with argon for 5 min and heated at 155° C. for 16 h in a closed vial. After cooling, the reaction mixture was poured into water and extracted with ethyl acetate. The organic layer was dried over MgSO4 and evaporated. Flash chromatography (2 g silica gel, 10 to 30% ethyl acetate in heptane) yielded a white solid (22 mg, 52%), MS (ISP): 354.3 ([M+H]+).
WORKUP
后处理
- customThe mixture was degassed with argon for 5 min
- temperatureAfter cooling
- additionthe reaction mixture was poured into water
- extractionextracted with ethyl acetate
- dry with materialThe organic layer was dried over MgSO4
- customevaporated