Triethylamine → 6-((2R,5S)-2,5-Dimethyl-piperazin-1-yl)-nicotinonitrile
반응식
[CH3:1][C@H:2]1[CH2:7][NH:6][C@H:5]([CH3:8])[CH2:4][NH:3]1.Cl[C:10]1[CH:17]=[CH:16][C:13]([C:14]#[N:15])=[CH:12][N:11]=1.C(N(CC)CC)C>CN1CCCC1=O>[CH3:1][C@@H:2]1[CH2:7][NH:6][C@@H:5]([CH3:8])[CH2:4][N:3]1[C:10]1[CH:17]=[CH:16][C:13]([C:14]#[N:15])=[CH:12][N:11]=1참가 물질
5
실험 절차
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)
후처리
- customMicrowave reaction mixture for 30 min at 150° C
- customPartition between ethyl acetate and water
- customcollecting organic phase
- dry with materialDry with sodium sulfate
- filtrationfilter
- concentrationconcentrate
- customPurify on preparative HPLC
출처 및 근거
- ORD 기록
- ord-bc5f400ac57641de862139b65cf0bb17
- 출처 데이터셋
- uspto-grants-2013_09
- 특허 번호
- US08536168B2
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