Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → 6-((2R,5S)-2,5-Dimethyl-piperazin-1-yl)-nicotinonitrile
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 2,5-Dimethylpiperazine, trans- | HCID 220672 | — |
| 반응물 | 6-Chloro-3-pyridinecarbonitrile | HCID 5152094 | — |
| 용매 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 생성물 | 6-((2R,5S)-2,5-Dimethyl-piperazin-1-yl)-nicotinonitrile | HCID 57471610 | 9% |
반응 단계
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)
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08536168B2 |
| 출처 데이터셋 | uspto-grants-2013_09 |
| ORD ID | ord-bc5f400ac57641de862139b65cf0bb17 |
| 출처 메모 | uspto-grants-2013_09 |