HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylamine → 6-((2R,5S)-2,5-Dimethyl-piperazin-1-yl)-nicotinonitrile
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | 2,5-Dimethylpiperazine, trans- | HCID 220672 | — |
| Edukt | 6-Chloro-3-pyridinecarbonitrile | HCID 5152094 | — |
| Lösungsmittel | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Produkt | 6-((2R,5S)-2,5-Dimethyl-piperazin-1-yl)-nicotinonitrile | HCID 57471610 | 9% |
Reaktionsschritte
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)
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08536168B2 |
| Quelldatensatz | uspto-grants-2013_09 |
| ORD ID | ord-bc5f400ac57641de862139b65cf0bb17 |
| Quellennotiz | uspto-grants-2013_09 |