反应详情

温度

50 °C

A yellow solution of N-([1,1′-biphenyl]-3-ylmethyl)-N-(1-(4-fluoro-2,6-dimethoxyphenyl)but-3-en-1-yl)acrylamide (152 mg; 0.34 mmol; 1.0 equiv.) in anh. DCM (17 ml) was treated with titanium(IV) isopropoxide (0.20 ml; 0.68 mmol; 2.0 equiv.), and the mixture was heated to 50° C., under nitrogen, for 1 h. Benzylidene-bis(tricyclohexylphosphine)dichlororuthenium (11.3 mg; 0.04 equiv.) was then added, and the resulting mixture was further heated at reflux for 20 h. Subsequent concentration to dryness under reduced pressure, and purification by FC (DCM/MeOH=50/1) afforded 1-([1,1′-biphenyl]-3-ylmethyl)-6-(4-fluoro-2,6-dimethoxyphenyl)-5,6-dihydropyridin-2(1H)-one as a pale yellow foam. LC-MS (conditions A): tR=0.94 min.; [M+H]+: 417.76 g/mol.

1. temperaturethe resulting mixture was further heated
2. temperatureat reflux for 20 h
3. concentrationSubsequent concentration to dryness
4. customunder reduced pressure, and purification by FC (DCM/MeOH=50/1)