化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → (R)-6-(3-Methylpiperazin-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 | Triethylamine hydrochloride | HCID 11130 | — |
| 反応物 | 6-Chloro-3-pyridinecarbonitrile | HCID 5152094 | — |
| 反応物 | 2-Methylpiperazine, (R)- | HCID 7330434 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | (R)-6-(3-Methylpiperazin-1-yl)nicotinonitrile | HCID 44186481 | 59% |
反応手順
Triethylamine (5.51 g, 4 mL, 54.6 mmol, 2.7 eq) is added to a solution of 6-chloro-nicotinonitrile (2.76 g, 20 mmol, 1 eq), (R)-2-methyl-piperazine (2.00 g, 20 mmol, 1 eq) in DMF (15 mL), and the resulting solution is stirred at rt for 36 h. A white precipitate of triethylamine hydrochloride forms in the course of the reaction. Water (15 mL) and EtOAc (100 mL) are added, the organic layer is separated, dried over sodium sulfate and concentrated under reduced pressure to a white residue. The solid is further dried under high vacuum to yield the desired product as a white solid (2.3 g, 59%).
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-60167e6f1e81401bbd6452b0dc756490 |
| 出典メモ | uspto-grants-2013_09 |