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Acetic Acid → 5-bromo-N-(pyridin-2-yl)thiazol-2-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | N-(pyridin-2-yl)thiazol-2-amine | HCID 956683 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 5-bromo-N-(pyridin-2-yl)thiazol-2-amine | HCID 5329400 | — |
反応手順
To a flask containing pyridin-2-yl-thiazol-2-yl-amine (5-2, 3.92 g, 0.0221 mol) was added acetic acid. Bromine (1.14 mL, 0.0221 mol) was then added dropwise to the stirred solution at ambient temperature. The reaction was stirred for 15 min, resulting in an orange-white precipitate. At 15 min, 100 mL H2O were added and solid NaHCO3 introduced, causing a large amount of foaming. The product was obtained as a tan colored precipitate, which was washed with 1.5 L H2O and dried under high vacuum overnight. 1H NMR (DMSO-d6): δ11.53 (bs, 1H), 8.31 (d, 1H, J=3.3 Hz), 7.73 (t, 1H, J=7.6 Hz), 7.45 (s, 1H), 7.05 (d, 1H, J=8.4 Hz), 6.96 (t, 1H, J=5.5 Hz). Mp: 210-212° C. (dec). [M+H]+=255.9.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06586423B2 |
| 出典データセット | uspto-grants-2003_07 |
| ORD ID | ord-7ecf22ce74554acba20c68a61e7807b9 |
| 出典メモ | uspto-grants-2003_07 |