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CAS No. : | 41110-33-2 | MDL No. : | MFCD04116910 |
Formula : | C7H8N2O2 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | CRBOSZMVDHYLJE-UHFFFAOYSA-N |
M.W : | 152.15 | Pubchem ID : | 465065 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | |
Hazard Statements: | H315-H319-H335 | Packing Group: | |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
46% | With bromine; acetic acid; at 80℃; for 1h; | [0115j To a solution of methyl 5-methylpyrazine-2-carboxylate (0.5 g, 3.28 mmol) in acetic acid (5 ml) was added bromine (0.i9 ml, 3.6i mmol) at room temperature. The reaction mixture was heated at 80C for 45 mm. The reaction mixture was concentrated to remove acetic acid. The residue was basified with saturated sodium bicarbonate solution and extracted with ethyl acetate. The organic layer was dried and concentrated. The crude was purified by silica gel column chromatography using 20% ethyl acetate in hexane to afford the title compound methyl 5-(bromomethyl)pyrazine-2-carboxylate (0.3 g, 40%) as a brownish liquid. Calculated M+H: 230.97; Found M+H: 231.0. |
32.9% | With N-Bromosuccinimide; 2,2'-azobis(isobutyronitrile); In tetrachloromethane; for 10h;Reflux; | A mixture of methyl 5-methylpyrazine-2-carboxylate (3.000 g, 19.7 17 mmol),1 -bromopyrrolidine-2,5-dione (NB S, 3.685 g, 20.703 mmol) and Azobisisobutyronitrile (AIBN, 1.295 g, 7.887 mmol) in carbon tetrachioride (20 mL) prepared at theroom temperature was heated at reflux for 10 hr, and cooled down to the ambient temperature. Then, water was added to the reaction mixture, followed by extraction withethyl acetate. The organic layer was washed with aqueous saturated sodium chloridesolution, dried with anhydrous MgSO4, filtered, and concentrated in vacuo. The residuewas chromatographed (Si02, 40 g cartridge; ethyl acetate / hexane = 0 % to 15 %) togive methyl 5-(bromomethyl)pyrazine-2-carboxylate as gray solid (1.500 g, 32.9 %). |
With N-Bromosuccinimide; 2,2'-azobis(isobutyronitrile); In tetrachloromethane; at 70℃; for 20h; | Synthesis Example 13-2: Synthesis of 5-bromomethyl-2-methoxy carbonyl pyrazine (Compound IV-3) 500 mg of the compound obtained in Synthesis Example 13-1 was dissolved in 10 ml of carbon tetrachloride, and then 585 mg of N-bromosuccinimide and 54 mg of azobisisobutyronitrile were added to the solution. After the solution was stirred in oil bath for 20 hours at 70C, the reaction solution was filtrated, and then the filtrate was then concentrated. The resulting residue was purified by means of silica gel column chromatography (14 g, chloroform/ethyl acetate= 2/1), and 328.7mg of the above-mentioned compound was obtained as light-yellow syrup. MS(EI,Pos.):m/z=229,231[M+1]+ 1H-NMR(500MHz,DMSO-d6): delta=4.06 (3H,s), 4.62 (2H,s), 8.83 (1H,d,J=1. 5Hz), 9.26 (1H,d,J=1.5Hz). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In tetrachloromethane; | Example 13-2 Synthesis of 5-bromomethyl-2-methoxycarbonylpyrazine (Compound IV-3) The compound obtained in Example 13-1 (500 mg) was dissolved in carbontetrachloride (10 ml) and N-bromosuccinimido (585 mg) and azobisisobutylonitrile (54 mg) were added. After stirring for 20 hours over an oil bath at 70C, the reaction mixture was filtered and the filtrate was concentrated. The residue was purified by silica gel column chromatography (14 g, chloroform/ethyl acetate = 2/1) to obtain the title compound (328.7 mg) as pale yellow syrup. MS(EI,Pos.):m/z=229,231[M+1]+ 1H-NMR(500MHz,DMSO-d6):delta=4.06(3H,s),4.62(2H,s),8.83(1H,d, J=1.5Hz),9.26(1H,d,J=1.5Hz). |
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