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Sodium Carbonate → 1-(2-(Piperazin-1-yl)pyrimidin-5-yl)ethanone hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 2,2,2-Trifluoroethyl Acetate | HCID 136256 | — |
| 反応物 | Butyl 4-(5-acetylpyrimidin-2-yl)piperazine-1-carboxylate | HCID 131735539 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(2-(Piperazin-1-yl)pyrimidin-5-yl)ethanone hydrochloride | HCID 118022442 | 86% |
反応手順
To a solution of -butyl 4-(5-acetylpyrimidin-2-yl)piperazine-1-carboxylate (4.5 g, 14.7 mmol) in dichloromethane (80 mL) was added trifluoroethyl acetate (20 mL), and the mixture was stirred at RT for 3 h. LCMS showed the reaction was completed. The reaction mixture was neutralized with sodium carbonate solution and extracted with dichloromethane. The organic layer was dried over sodium sulfate, filtered and concentrated to afford the title compound as a light yellow solid (2.6 g, 86%), which was directly used in the next step without further purification. MS (ES+) C10H14N4O requires: 206, found: 207 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09334263B2 |
| 出典データセット | uspto-grants-2016_05 |
| ORD ID | ord-18eeb75877ba4bc0afdcd367ba7b7565 |
| 出典メモ | uspto-grants-2016_05 |