Lawesson's reagent → 6-bromo-5-chloro-3,4-dihydroquinoline-2(1H)-thione
反応式
[Br:1][C:2]1[C:3]([Cl:13])=[C:4]2[C:9](=[CH:10][CH:11]=1)[NH:8][C:7](=O)[CH2:6][CH2:5]2.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:23])=CC=1>C1(C)C=CC=CC=1>[Br:1][C:2]1[C:3]([Cl:13])=[C:4]2[C:9](=[CH:10][CH:11]=1)[NH:8][C:7](=[S:23])[CH2:6][CH2:5]2参加物
4
反応条件
- 温度
- 100 °C
実験手順
To a stirred solution of 6-bromo-5-chloro-3,4-dihydroquinolin-2(1H)-one (143-5; 1.2 g, 0.0046 mol) in toluene (20 mL) was added Lawesson's reagent (1.8 g, 0.0046 mol). Reaction mass was refluxed at 100° C. for 12 h. The reaction mixture was concentrated and directly purified by silica gel column chromatography to obtain title compound 6-bromo-5-chloro-3,4-dihydroquinoline-2(1H)-thione. MS (M+1): 277.8.
後処理
- customReaction mass
- concentrationThe reaction mixture was concentrated
- customdirectly purified by silica gel column chromatography
出典と根拠
- ORDレコード
- ord-4a10e994832a43059918077d6957d353
- 出典データセット
- uspto-grants-2015_07
- 特許番号
- US09073929B2
反応ノート
読み込み中…