METHYL 6-BROMO-3-METHOXYPYRAZINE-2-CARBOXYLATE synthesis
- Product Name:METHYL 6-BROMO-3-METHOXYPYRAZINE-2-CARBOXYLATE
- CAS Number:259794-06-4
- Molecular formula:C7H7BrN2O3
- Molecular Weight:247.05
Yield:-
Reaction Conditions:
Stage #1: methyl 3-amino-6-bromopyrazine-2-carboxylatewith sulfuric acid;sodium nitrite at 0; for 0.5 h;
Stage #2: methanol for 5 h;Reflux;
Steps:
162.1
To a solution of methyl 3-amino-6-bromopyrazine-2-carboxylate (1.00 g, 4.31 mmol) in cone. H2SO4 (5.9 mL) at 0 °C was added NaN02 (0.60 g, 8.6 mmol) in one rapid portion. The resulting mixture was stirred at 0 °C for 30 minutes and then poured into 53 mL of MeOH. The combined mixture was then heated at reflux for 5 hrs. After cooling to RT and removal of the volatiles in vacuo, the resulting residue was taken up in ice-cold water and extracted with chloroform. The combined organic extracts were then washed sequentially with saturated aq. NaHCOs solution and water, dried over Na2SO i, filtered and the filtrate concentrated in vacuo. Further purification by way of column chromatography (S1O2, gradient elution, Hex -^ 1 :1 Hex:EtOAc) furnished methyl 6-bromo-3-methoxypyrazine-2-carboxylate.
References:
WO2013/134562,2013,A1 Location in patent:Paragraph 00362
6966-01-4
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259794-06-4
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