化工社化工社 化学情報印刷レポート · 研究参考用
1,2-Dichloroethane → 1-[4-(Pyrimidin-2-ylaminomethyl)-piperidin-1-yl]4-thiophen-2-yl-butan-1-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,2-Dichloroethane | HCID 11 | — |
| 反応物 | Piperidine | HCID 8082 | — |
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | 4-(2-Thienyl)Butyric Acid | HCID 78386 | — |
| 反応物 | Benzyl 4-[(2-pyrimidinylamino)methyl]-1-piperidinecarboxylate | HCID 9923385 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-[4-(Pyrimidin-2-ylaminomethyl)-piperidin-1-yl]4-thiophen-2-yl-butan-1-one | HCID 22135671 | — |
反応手順
Benzyl 4-[(2-pyrimidinylamino)methyl]-1-piperidinecarboxylate (EXAMPLE 16) was hydrogenated as described in EXAMPLE 30, Step 1. The resulting piperidine was combined with EDC (1.3 equiv.), HOBT (1.0 equiv.), and 4-thiophen-2-yl-butyric acid (1.0 equiv.) in DMF and stirred for 2 h. The resulting reaction solution was partitioned into ethyl acetate and aqueous sodium bicarbonate. The organic layer was seperated and washed with pH 4.5 citric acid buffer (10% citric acid and sodium hydroxide), dried (sodium sulfate), and concentrated to yield the desired 1-[4-(pyrimidin-2-ylaminomethyl)-piperidin-1-yl]-4-thiophen-2-yl-butan-1-one. M.S. (M+1): 345.25.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07053089B2 |
| 出典データセット | uspto-grants-2006_05 |
| ORD ID | ord-8dcdaf91dbe64bf3bea6fcb554481fdb |
| 出典メモ | uspto-grants-2006_05 |