反应详情

To a solution of XXIII (2.7 g, 10.9 mmol) in THF was added dropwise a solution of pyridinium tribromide (3.83, 0.41 mmol) in 50 mL of THF at rt. The reaction mixture was stirred for 15 min before 60 mL of water was added into the flask. The aqueous phase was extracted with EtOAc. The combined organic phase was washed with saturated NaCl, dried over Na2SO4 and concentrated. The residue was purified by flash silica gel chromatography to give (6-bromo-1,2,3,4-tetrahydro-quinoline-3-yl)-carbamic acid tert-butyl ester XXIV (2.5 g, 70%) as white solid.

1. additionwas added into the flask
2. extractionThe aqueous phase was extracted with EtOAc
3. washThe combined organic phase was washed with saturated NaCl
4. dry with materialdried over Na2SO4
5. concentrationconcentrated
6. customThe residue was purified by flash silica gel chromatography