関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Dimethylformamide dimethyl acetal | HCID 78373 | — |
| 反応物 | t-Butyl 5-methylpyrazine-2-carboxylate | HCID 57475683 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | t-butyl 5-((E)-2-dimethylaminovinyl)pyrazine-2-carboxylate | HCID 57475684 | — |
反応手順
A mixture of t-butyl 5-methylpyrazine-2-carboxylate (1.35 g), DMF (25 mL) and N,N-dimethylformamide dimethylacetal (25 mL) was stirred at 130° C. for 5 h. The reaction solution was cooled to RT and diluted with EtOAc. The mixture was washed with a saturated NaCl solution three times. The organic layer was dried over anhydrous MgSO4, and the insoluble matter was separated by filtration. The filtrate was concentrated and the residue was purified by silica gel column chromatography to obtain the title compound (648 mg). 1H-NMR (CDCl3) δ (ppm): 1.63 (s, 9H), 3.00 (s, 6H), 5.16 (d, J=12.8 Hz, 1H), 7.72 (d, J=12.8 Hz, 1 H), 8.16 (d, J=1.2 Hz, 1H), 8.81 (d, J=1.6 Hz, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08940734B2 |
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| 出典データセット | uspto-grants-2015_01 |
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| ORD ID | ord-11f0504771a747e79eb33b206549c666 |
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| 出典メモ | uspto-grants-2015_01 |
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