3-Acetylaminoquinoline → N-(1,2,3,4-tetrahydroquinolin-3-yl)acetamide
反応式
[C:1]([NH:4][C:5]1[CH:6]=[N:7][C:8]2[C:13]([CH:14]=1)=[CH:12][CH:11]=[CH:10][CH:9]=2)(=[O:3])[CH3:2].C(OCC)(=O)C.CCCCCC>C(O)C.[Pd]>[CH3:2][C:1]([NH:4][CH:5]1[CH2:14][C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[NH:7][CH2:6]1)=[O:3]参加物
5
実験手順
300 mg of the 3-(acetylamino)quinoline (Rf (D)=0.43) obtained by a single recrystallization from ethyl acetate/hexane are hydrogenated in 10 ml of ethanol in the presence of 60 mg of palladium-on-charcoal (10% of Pd) at 50° C. under normal pressure for 20 h. After the reaction mixture has been filtered over Celite® 545 and the crude product has been purified by chromatography over 25 g of silica gel (mobile phase P), 3(R,S)-methylcarbonylamino-1,2,3,4-tetrahydroquinoline is obtained: Rf (P)=0.49; MS: (M)+ =190.
後処理
- filtrationAfter the reaction mixture has been filtered over Celite® 545
- customthe crude product has been purified by chromatography over 25 g of silica gel (mobile phase P)
出典と根拠
- ORDレコード
- ord-b6c27f62036443d4b365dedab9fc3976
- 出典データセット
- uspto-grants-1998_02
- 特許番号
- US05719141
反応ノート
読み込み中…