Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → (R)-6-(3-Methylpiperazin-1-yl)nicotinonitrile
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Triethylamine hydrochloride | HCID 11130 | — |
| 반응물 | 6-Chloro-3-pyridinecarbonitrile | HCID 5152094 | — |
| 반응물 | 2-Methylpiperazine, (R)- | HCID 7330434 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | (R)-6-(3-Methylpiperazin-1-yl)nicotinonitrile | HCID 44186481 | 59% |
반응 단계
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%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08536168B2 |
| 출처 데이터셋 | uspto-grants-2013_09 |
| ORD ID | ord-60167e6f1e81401bbd6452b0dc756490 |
| 출처 메모 | uspto-grants-2013_09 |