関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitric Acid | HCID 944 | — |
| 反応物 | 7-Bromo-2-ethylpyrazolo[1,5-a]pyridine | HCID 21984510 | — |
| 溶媒 | Sulfuric Acid | HCID 1118 | — |
| 生成物 | 7-Bromo-2-ethyl-3-nitropyrazolo[1,5-a]pyridine | HCID 21984481 | 31% |
反応手順
Fuming nitric acid (1.7 mL) was added dropwise to a solution of 7-bromo-2-ethylpyrazolo[1,5-a]pyridine (6.9 g, 34.2 mmol) in concentrated sulfuric acid (13.8 mL) at an internal temperature of below 30° C. while cooling with ice. After stirring the reaction mixture for 30 minutes, it was added to ice water (138 mL) and the precipitate was filtered out. The obtained precipitate was added ethyl acetate (226 mL) and methanol (38 mL), and the mixture was heated to 70° C., and then the precipitate was collected by filtration while cooling with ice. The solvent of the obtained filtrate was evaporated under reduced pressure, and the concentrated residue was recrystallized from heptane-ethyl acetate (1:1) to afford 2.4 g of the title compound as light brown crystals (31% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07176216B2 |
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| 出典データセット | uspto-grants-2007_02 |
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| ORD ID | ord-8b5b93c95e944199a78f70e5b9b2c00b |
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| 出典メモ | uspto-grants-2007_02 |
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