Triethylamine → 6-((2R,5S)-2,5-Dimethyl-piperazin-1-yl)-nicotinonitrile
反応式
[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]=1参加物
5
実験手順
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)
後処理
- 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
出典と根拠
- ORDレコード
- ord-bc5f400ac57641de862139b65cf0bb17
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08536168B2
反応ノート
読み込み中…