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Hydrochloric Acid → 4-Chloro-6-(indolin-1-yl)pyrimidin-5-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Indoline | HCID 10328 | — |
| 反応物 | 5-Amino-4,6-dichloropyrimidine | HCID 79434 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-Chloro-6-(indolin-1-yl)pyrimidin-5-amine | HCID 23477456 | 34.4% |
反応手順
To a stirring slurry of 5-amino-4,6-dichloropyrimidine (3 g, 18.29 mmol) and indoline (2.057 mL, 18.29 mmol) in ethanol (7 mL) and water (43 mL) was added concentrated aqueous HCl (600 μL) and the mixture was refluxed for 3 h and left to stir at room temperature overnight. The reaction mixture was extracted with ethyl acetate, washed with water, brine, dried over MgSO4 and solvent evaporated. The resulting residue was triturated in 25% ethyl acetate in hexanes for 1 h then filtered to afford title compound 105 (1.55 g, 34%) as a tan solid. LRMS (ESI): (calc) 246.07 (found) 247.2 (MH)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08399452B2 |
| 出典データセット | uspto-grants-2013_03 |
| ORD ID | ord-08f40fd5706e41b38553fabd87bac416 |
| 出典メモ | uspto-grants-2013_03 |