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Diisopropylethylamine → 1-Pyrimidin-2-yl-piperidine-4-carboxylic acid N'-(3-methyl-butyryl)-hydrazide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 反応物 | 1-(Pyrimidin-2-yl)piperidine-4-carboxylic acid | HCID 2767267 | — |
| 反応物 | 1-Hydroxybenzotriazole hydrate | HCID 2796029 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-Pyrimidin-2-yl-piperidine-4-carboxylic acid N'-(3-methyl-butyryl)-hydrazide | HCID 23544067 | 46.4% |
反応手順
The residue was added to a mixture of 1-pyrimidin-2-yl-piperidine-4-carboxylic acid (6.6 g, 31.7 mmol) (see reference U.S. Pat. No. 4,826,843), 1-hydroxybenzotriazole hydrate (4.28 g, 31.7 mmol) and 1-(3-dimethylaminopropyl-3-ethylcarbodiimide hydrochloride (6.09 g, 31.7 mmol) in dichloromethane (50 ml). Diisopropylethylamine (17 ml, 95 mmol) was added and the mixture was stirred for 3 days. The solvent was evaporated and the residue was triturated with water and then with diethyl ether to give the title compound as a white solid (4.49 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07084145B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-4c0cc20436e440c9a6f5ae1c9ddc1270 |
| 出典メモ | uspto-grants-2006_08 |