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Bromocyclopentane → 1-cyclopentyl-4-iodo-1H-pyrazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Bromocyclopentane | HCID 8728 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Iodopyrazole | HCID 77022 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-cyclopentyl-4-iodo-1H-pyrazole | HCID 56777330 | 89.5% |
反応手順
To a solution of 4-iodo-1H-pyrazole (5 g, 25.78 mmol, 1.0 eq.) in DMF (25 ml) were added K2CO3 (8.908 g, 64.45 mmol, 2.5 eq.) and bromocyclopentane (4.96 g, 33.51 mmol, 1.3 eq.). The mixture was stirred at RT for 12 h. The mixture was quenched and extracted as in Intermediate Example 5(a). The solvent was distilled off to give the product in 89.5% yield. 1H NMR (300 MHz, CDCl3): δ 7.49 (s, 1H), 7.45 (s, 1H), 4.66-4.62 (m, 1H), 2.17-2.02 (m, 1H), 2.00-1.96 (m, 2H), 1.93-1.78 (m, 2H), 1.73-1.67 (m, 2H). LC-MS (ESI): Calculated mass: 262; Observed mass: 263 [M+H]+ (rt: 1.57 min).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09447091B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-58880dbf79124678b073a50a8366605f |
| 出典メモ | uspto-grants-2016_09 |