8-bromo-6-nitroquinoline synthesis
- Product Name:8-bromo-6-nitroquinoline
- CAS Number:120287-30-1
- Molecular formula:C9H5BrN2O2
- Molecular Weight:253.05
Yield: 28% ， 4%
Reaction Conditions:
with N-Bromosuccinimide;acetic acid at 50; for 17 h;
Steps:
A1.a Preparation of intermediates 1 and 2
A solution of 6-nitroquinoline (28.1 g; 161 mmol) and A/-bromosuccinimide (28.7 g; 161 mmol) in acetic acid (280 ml) was heated at 50°C for 17 hours. The precipitate solid was filtered and washed with Et20, water and then Et20 to afford 14.7g g (27%) of intermediate 2 (purity 93%) . The organic layer was evaporated to dryness and the residue was purified by chromatography over silica gel (mobile phase gradient from 50% petroleum ether, 50% DCM to 100% DCM). The pure fractions were collected and the solvent was evaporated, yielding 2.25 g (4 %) of intermediate 2 and 16.6g of a residue that was submitted to a second purification by chromatography over silica gel (mobile phase 50% petroleum9/1/0.2 cyclohexane/ diethyl ether/ DCM). The pure fractions were collected and the solvent was evaporated, yielding 14.1 g (28%) of intermediate 1.
References:
ASTEX THERAPEUTICS LIMITED;BERDINI, Valerio;ANGIBAUD, Patrick René;WOODHEAD, Steven John;SAXTY, Gordon WO2013/61074, 2013, A1 Location in patent:Page/Page column 147
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