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7-bromopyrido[3,4-b]pyrazine-2,3(1H,4H)-dione hydrochloride[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
With hydrogenchloride; In water; at 120℃; for 14h;
[0287] Reference V -bromo-2,3-dichloropyrido[3,4-b]pyrazine [0290] Step 1 : 7-bromopyrido[3,4-b]pyrazine-2,3(lH,4H)-dione hydrochloride [0291] To a solution of <strong>[1033203-41-6]6-bromopyridine-3,4-diamine</strong> (467 mg, 2.484 mmol) in HC1 (3726 mu, 14.90 mmol, 4 M aq) was added oxalic acid (257 mg, 2.86 mmol). The mixture was heated at 120 C for 14 h then filtered, washed with cold water and dried under vacuum to yield the title compound as a tan solid.
A mixture of <strong>[1033203-41-6]6-bromopyridine-3,4-diamine</strong> (100 mg, 0.53 mmol) and lH-pyrazole-4-carboxylic acid (60 mg, 0.53 mmol) in polyphosphoric acid (1 g) was heated in a sealed vial at 200 °C for 18 h. The reaction mixture was diluted with water and made basic by addition of NaOH (50percent aq.) and a white precipitate formed. The solid thus formed was collected by filtration and washed with water to afford the title compound (150mg, quant.). LCMS (ESI): [M+H]+ 264.1.
2-Bromo-5-nitropyridin-4-amine (300.0 mg, 2.48 mmol) and Fe (300.0 mg, 5.37 mmol) were added to AcOH, and the reaction mixture was stirred at 75 C. for 4 hours and then cooled to room temperature. The reaction mixture was filtered through celite and then concentrated under reduced pressure. The residue was purified by column chromatography (n-Hex:EtOAc=50:50) on amine silica. The fractions containing the product were collected and concentrated to obtain brown solid compound of 6-bromopyridine-3,4-diamine (200.0 mg, 78%). [1234] 1H-NMR (400 MHz, DMSO-d6); delta: 7.39 (s, 1H), 6.42 (s, 1H), 5.74 (brs, 2H), 4.66 (brs, 2H)
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