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2-Bromopropane → 4-Bromo-1-isopropyl-1H-pyrazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Bromopropane | HCID 6358 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Bromopyrazole | HCID 16375 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-Bromo-1-isopropyl-1H-pyrazole | HCID 22329200 | 89% |
反応手順
To a solution of 4-bromo-1H-pyrazole (5 g, 34 mmol) in DMF (70 ml) were added K2CO3 (11.83 g, 85.6 mmol, 2.5 eq.) and 2-bromopropane (6.3 g, 51.36 mmol, 1.5 eq.) and 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 and the crude residue was purified by column chromatography (60-120 silica gel, 20% ethyl acetate in hexane) to afford the product in 89% yield (5.8 g). 1H NMR (300 MHz, DMSO-d6): δ 8.01 (s, 1H), 7.50 (s, 1H), 4.49-4.43 (m, 1H), 1.38 (d, 6H).
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-27cb84df084c4cb9be2332bc6cd068a1 |
| 出典メモ | uspto-grants-2016_09 |