反应详情

温度

100 °C

To a 150 mL flask containing 6-bromo-1′-methyl-2′,3′,5′,6′-tetrahydro-1′H-[2,4′]bipyridinyl-4′-ol (5 g, 18.5 mmol) was added conc. H2SO4 (50 mL). Heated to 100° C. for 18 h. Cooled and poured onto ice carefully. Neutralized with 5 N NaOH and extracted with EtOAc. Washed with brine, dried (MgSO4) and concentrated in vacuo. Diluted residue with EtOAc and filtered. Concentrated filtrate in vacuo to give 6-bromo-1′-methyl-1′,2′,3′,6′-tetrahydro-[2,4′]bipyridinyl as an orange oil. MS m/z: 254.2 (M+H). Calc'd for C11H13BrN2 253.14.

1. temperatureCooled
2. additionpoured onto ice carefully
3. extractionNeutralized with 5 N NaOH and extracted with EtOAc
4. washWashed with brine
5. dry with materialdried (MgSO4)
6. concentrationconcentrated in vacuo
7. filtrationDiluted residue with EtOAc and filtered