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Pyridine → 4-Nitro-1-p-tolyl-1H-pyrazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | 4-nitro-1H-pyrazole | HCID 16376 | — |
| 反応物 | Tolylboronic acid | HCID 79799 | — |
| 触媒 | Cupric acetate | HCID 8895 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-Nitro-1-p-tolyl-1H-pyrazole | HCID 11413030 | 31% |
反応手順
To 4-tolylboronic acid (544 mg, 4.00 mmol), 4-nitropyrazole (226 mg, 2.00 mmol), copper (II) acetate (545 mg, 3.00 mmol), and 4 Å sieves (1.5 g) in DCM (15 mL), was added pyridine (0.32 mL, 4 mmol) at RT, and stirred for 5 h. The mixture was filtered through Celite, washing with DCM, then evaporated to dryness. The residue was purified by FCC, eluting with 0-30% ethyl acetate in cyclohexane, to give the title compound as a white solid (126 mg, 31%). LCMS (Method 3): Rt 3.93 min, m/z 204.1 [MH−].
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08835431B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-b77fbc78aea049efbe40ef84e64179be |
| 出典メモ | uspto-grants-2014_09 |