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
- 120 °C
PROCEDURE
实验过程
To a solution of 1-phenyl-1,2,3,6-tetrahydropyridin-4-yl trifluoromethanesulfonate (104 mg, 0.339 mmol) in 1,4-Dioxane (3 ml) and H2O (1 ml) were added 5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)indolin-2-one (97.6 mg, 0.377 mmol), Pd(PPh3)4 (38.8 mg, 0.00336 mmol), LiCl (47.1 mg, 1.11 mmol) and K2CO3 (140 mg, 1.01 mmol). After stirring at 120° C. in microwave reactor for 1 h, the reaction mixture was quenched by sat. NaHCO3 aq. The resulting mixture was extracted with CHCl3, the organic layer was washed with brine, dried over Na2SO4 and concentrated. The residue was purified by column chromatography (CHCl3/MeOH) to give 5-(1-phenyl-1,2,3,6-tetrahydropyridin-4-yl)indolin-2-one (75.8 mg) as mixture of triphenylphosphine oxide.
WORKUP
后处理
- customthe reaction mixture was quenched by sat. NaHCO3 aq. The resulting mixture
- extractionwas extracted with CHCl3
- washthe organic layer was washed with brine
- dry with materialdried over Na2SO4
- concentrationconcentrated
- customThe residue was purified by column chromatography (CHCl3/MeOH)