反应详情

N,N-dimethylbarbituric acid (420 mg) and Pd(PPh3)4 (117 mg) were added to a solution of 3-(2-chloro-4-diallylamino-phenyl)-2-(2-chloro-pyridin-4-yl)-1,1,1-trifluoro-butan-2-ol (300 mg) in DCM (60 ml). The mixture was heated under reflux for 3 h. 1N aqueous NaOH solution was added and extracted with DCM. The combined organic layers were dried over Na2SO4 and then concentrated to an oil. The residue was purified by flash chromatography (SiO2, 0 to 50% EtOAc/heptane) to give the title compound (170 mg) as light yellow foam. MS (m/e)=365.0 [M+H+].

1. temperatureThe mixture was heated
2. temperatureunder reflux for 3 h
3. extractionextracted with DCM
4. dry with materialThe combined organic layers were dried over Na2SO4
5. concentrationconcentrated to an oil
6. customThe residue was purified by flash chromatography (SiO2, 0 to 50% EtOAc/heptane)