関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-Bromo-1-propanol | HCID 12308 | — |
| 反応物 | 4-nitro-1H-pyrazole | HCID 16376 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 3-(4-Nitro-pyrazol-1-yl)-propan-1-ol | HCID 19621837 | 93% |
反応手順
To a stirred solution of 4-nitro-1H-pyrazole (27) (1.0 g, 8.9 mmol) in MeCN (15 mL) was added K2CO3 (1.8 g, 13.2 mmol) and 3-bromo-propanol (880 μL, 9.7 mmol). The mixture was stirred at 75° C. for 6 hours. The solvent was evaporated in vacuo and the residue partitioned between H2O (15 mL) and EtOAc (15 mL). The layers were separated and the aqueous phase extracted with EtOAc (2×15 mL). The combined organics were dried (MgSO4), filtered and the solvent evaporated in vacuo to afford the title compound as a pale yellow oil (1.41 g, 93%); LCMS, Rt=1.31 min (MeOH-FA method), m/z 172 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09433622B2 |
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| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-5832e3deb7e74ffd9ceb999f45ff1987 |
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| 出典メモ | uspto-grants-2016_09 |
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