反应详情

温度

100 °C

Bromine (750 μl, 14.6 mmol) in glacial acetic acid (5 ml) was added dropwise over 5 minutes to (6-benzyl-3,4,5,6,7,8-hexahydro-1H-[1,6]naphthyridin-2-one (3.37 g, 13.9 mmol) (reference WO9830560) dissolved in glacial acetic acid (50 ml) at 100° C. The mixture was heated at 100° C. for 2.5 hours and then was cooled to room temperature. The solvent was evaporated under reduced pressure and the residue was basified with 10% sodium carbonate solution (50 ml). The aqueous mixture was extracted with chloroform (4×50 ml) and the combined organic solutions were dried over sodium sulphate and evaporated under reduced pressure. The residue was purified by chromatography on silica gel using methanol in dichloromethane (gradient from 0:100 to 3:97) to give the title compound as yellow crystals (1.5 g).

1. temperaturewas cooled to room temperature
2. customThe solvent was evaporated under reduced pressure
3. extractionThe aqueous mixture was extracted with chloroform (4×50 ml)
4. dry with materialthe combined organic solutions were dried over sodium sulphate
5. customevaporated under reduced pressure
6. customThe residue was purified by chromatography on silica gel