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Sodium Bicarbonate → 2-(4-Methylthiazol-2-ylamino)pyridin-3-ol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 3-(Benzyloxy)-N-(4-Methyl-1,3-Thiazol-2-Yl)pyridin-2-Amine | HCID 16660015 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 生成物 | 2-(4-Methylthiazol-2-ylamino)pyridin-3-ol | HCID 10465616 | 78.5% |
反応手順
A 250 mL round-bottomed flask was charged 3-(benzyloxy)-N-(4-methylthiazol-2-yl)pyridin-2-amine (11.4 g, 38.3 mmol) in 6M HCl (100 mL), and the reaction mixture was heated to reflux for 10 hours. The reaction mixture was cooled to room temperature, poured onto ice and saturated sodium bicarbonate, filtered, dried under vacuum and triturated with hexanes to afford 2-(4-methylthiazol-2-ylamino)pyridin-3-ol (6.23 g, 78.5% yield) as a pale yellow solid. 1H NMR (CD3OD) δ 7.79 (dd, 1H), 7.07 (dd, 1H), 6.79 (dd, 1H), 6.46 (q, 1H), 2.28 (s, 3H). LCMS (5 to 95) Rt=2.69 min (apci) m/z=208 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08933077B2 |
| 出典データセット | uspto-grants-2015_01 |
| ORD ID | ord-ebd9e6fe969c487da022347defda37f7 |
| 出典メモ | uspto-grants-2015_01 |