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Triethylamine → 6-((2R,5S)-2,5-Dimethyl-piperazin-1-yl)-nicotinonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2,5-Dimethylpiperazine, trans- | HCID 220672 | — |
| 反応物 | 6-Chloro-3-pyridinecarbonitrile | HCID 5152094 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | 6-((2R,5S)-2,5-Dimethyl-piperazin-1-yl)-nicotinonitrile | HCID 57471610 | 9% |
反応手順
Combine (2S,5R)-2,5-dimethyl-piperazine (200 mg, 1.75 mmol), 6-chloro-nicotinonitrile (1.75 mmol) and triethylamine (5.25 mmol) in a 0.875 M solution of 1-methyl-2-pyrrolidinone. Microwave reaction mixture for 30 min at 150° C. Partition between ethyl acetate and water, collecting organic phase. Wash aqueous layer again with ethyl acetate and combine organics. Dry with sodium sulfate, filter and concentrate. Purify on preparative HPLC to give the title compound. (9% yield)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08536168B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-bc5f400ac57641de862139b65cf0bb17 |
| 出典メモ | uspto-grants-2013_09 |