反应详情

To a solution of 7-(1,3-dimethyl-1H-pyrazol-5-yl)-2,3,4,5-tetrahydro-1H-3-benzazepine (0.5 g) in dry THF (10 ml), diisopropylethylamine (0.85 ml) and 1-bromo-3-chloropropane (0.47 mL) were added and the resulting mixture was refluxed for 7 hours. After cooling at room temperature it was diluted with ethyl acetate (30 ml) washed twice with a saturated solution of NaHCO3 in water (20 ml), dried over Na2SO4 and concentrated under reduced pressure. The crude was purified by biotage chromatography using a silica 25 M+ cartridge and eluting with cHex/EtOAc 8:2 to give the title compound as a colourless oil (0.57 g).

1. temperaturethe resulting mixture was refluxed for 7 hours
2. washwashed twice with a saturated solution of NaHCO3 in water (20 ml)
3. dry with materialdried over Na2SO4
4. concentrationconcentrated under reduced pressure
5. customThe crude was purified by biotage chromatography
6. washeluting with cHex/EtOAc 8:2