反应详情

温度

60 °C

The compound of Example 169 (0.166 g) was dissolved in DMF (1 mL) and treated with palladium (II) acetate (0.007 g), 1,3-bis-diphenylphosphinopropane (0.012 g), triethylamine (0.1 mL) and ethanol (1 mL), and stirred at 60° C. for 18 hours under a CO balloon. The resulting solution was quenched with water, extracted with ethyl acetate, concentrated in vacuo, and purified by silica gel chromatography (87:10:3 ethyl acetate:methanol:triethylamine). The residue was further purified by chromatography on a reverse-phase solid-phase-extraction column, eluting with water-acetonitrile, 0.1% formic acid, to yield 0.114 g (73%) of the title compound.

1. customThe resulting solution was quenched with water
2. extractionextracted with ethyl acetate
3. concentrationconcentrated in vacuo
4. custompurified by silica gel chromatography (87:10:3 ethyl acetate:methanol:triethylamine)
5. customThe residue was further purified by chromatography on a reverse-phase solid-phase-extraction column
6. washeluting with water-acetonitrile, 0.1% formic acid