反应详情

温度

80 °C

Methanesulfonic acid (1.15 equiv.) was added to a stirred solution of ethyl 3-(6-oxo-1-phenyl-1,4,5,6-tetrahydropyridazin-3-yl)propanoate from Step 1 in n-propanol (1.1 M). The mixture was stirred overnight at 80° C. The mixture was cooled to rt and neutralized with aqueous 1 N NaOH (1 equiv.). Final mixture was concentrated under vacuum, diluted with toluene and concentrated again. The residue was purified by column chromatography on silica gel using a CombiFlashRF (Teledyne ISCO) eluting with EtOAc/Hex (0:100 to 60:40) to give the title compound (79%) as a brown oil.

1. concentrationFinal mixture was concentrated under vacuum
2. additiondiluted with toluene
3. concentrationconcentrated again
4. customThe residue was purified by column chromatography on silica gel using a CombiFlashRF (Teledyne ISCO)
5. washeluting with EtOAc/Hex (0:100 to 60:40)