N-bromobutanimide → HCID 59295129、化合物
反応式
[Cl:1][C:2]1[C:3]([NH:8][NH:9][C:10](=[O:15])[C:11]([F:14])([F:13])[F:12])=[N:4][CH:5]=[CH:6][N:7]=1.C1C(=O)N([Br:23])C(=O)C1>C(Cl)Cl.O>[Br:23][C:6]1[N:7]=[C:2]([Cl:1])[C:3]([NH:8][NH:9][C:10](=[O:15])[C:11]([F:12])([F:13])[F:14])=[N:4][CH:5]=1参加物
5
反応条件
- 温度
- -40 °C
実験手順
N′-(3-chloropyrazin-2-yl)-2,2,2-trifluoroacetohydrazide E-1 (19.5 g; 81.1 mmol) is dissolved in 300 ml anhydrous DCM and cooled down to −40° C. Afterwards NBS (18.8 g; 105 mmol) is added and stirred for 1 hour. The solution is diluted with water and extracted with DCM. The organic phase is then purified with flash chromatography: cHex/(EtOAc/CH3COOH=9/1)=80%/20% to 70%/30% within 10 column volumes.
後処理
- extractionextracted with DCM
- customThe organic phase is then purified with flash chromatography
出典と根拠
- ORDレコード
- ord-a166946e8f1141efba089a2aba4887b9
- 出典データセット
- uspto-grants-2016_02
- 特許番号
- US09266891B2
反応ノート
読み込み中…