関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl (6-bromo-2-nitropyridin-3-yloxy)acetate | HCID 59560649 | — |
| 触媒 | Iron | HCID 23925 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 6-Bromo-2H-pyrido[3,2-B][1,4]oxazin-3(4H)-one | HCID 21873772 | — |
反応手順
Ethyl (6-bromo-2-nitro-pyridin-3-yloxy)acetate (38 g, 0.125 mole) was dissolved in glacial AcOH (150 mL), and iron powder (20 g, 0.36 mole) was added. The mixture was mechanically stirred and heated at 90° C. for 5 h, then was cooled to room temperature and diluted with EtOAc (300 mL). The mixture was filtered through a pad of silica gel and the filtrate was concentrated in vacuo and the residue recrystallized from MeOH (15 g, 52%); MS (ES) m/z 229.0 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07592334B2 |
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| 出典データセット | uspto-grants-2009_09 |
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| ORD ID | ord-8d41c8066eea43c4b42faa2259e5399d |
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| 出典メモ | uspto-grants-2009_09 |
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