反应详情

A solution of 1,3-dimethylbarbituric acid ([CAS Reg. No. 769-42-6], 828 mg), tetrakis(triphenylphosphine) palladium (0) (230 mg) and 3-(2-Chloro-4-diallylamino-phenyl)-2-(2-chloro-pyridin-4-yl)-1,1,1-trifluoro-butan-2-ol (590 mg) in DCM (120 ml) was heated under reflux for 3 h. NaOH (1N aq) was added and extracted with DCM. The combined organic layers were dried over Na2SO4 and concentrated in vacuo. The residue was purified by flash chromatography (silica gel, ethyl acetate/heptane 0:100-50:50) to give the title compound as a light yellow gum (370 mg). MS (m/e)=365.0 [M+H+].

1. temperatureunder reflux for 3 h
2. extractionextracted with DCM
3. dry with materialThe combined organic layers were dried over Na2SO4
4. concentrationconcentrated in vacuo
5. customThe residue was purified by flash chromatography (silica gel, ethyl acetate/heptane 0:100-50:50)