Formic Acid → 1H-Imidazo[4,5-c]quinoline, 1-methyl-
反応式
[NH2:1][C:2]1[CH:3]=[N:4][C:5]2[C:10]([C:11]=1[NH:12][CH3:13])=[CH:9][CH:8]=[CH:7][CH:6]=2.[CH:14](O)=O>>[CH3:13][N:12]1[C:11]2[C:10]3[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=3[N:4]=[CH:3][C:2]=2[N:1]=[CH:14]1参加物
3
実験手順
A solution of 2.92 g of 3-amino-4-methylaminoquinoline (V-2) in 20 ml of formic acid was refluxed for 1.5 hours. The reaction mixture was concentrated under reduced pressure and the residue was partitioned between chloroform and saturated aqueous sodium hydrogen-carbonate. The organic layer was washed with brine and dried. The chloroform was removed and the residue was crystallized from n-hexane to give 2.39 g (yield: 77%) of the titled compound (II-2). This was recrystallized from ethyl acetate to give colorless crystals melting at 146°~148° C.
後処理
- concentrationThe reaction mixture was concentrated under reduced pressure
- customthe residue was partitioned between chloroform and saturated aqueous sodium hydrogen-carbonate
- washThe organic layer was washed with brine
- customdried
- customThe chloroform was removed
- customthe residue was crystallized from n-hexane
出典と根拠
- ORDレコード
- ord-17d6d76daa534459b5fbbf69d3be4f9a
- 出典データセット
- uspto-grants-1990_07
- 特許番号
- US04940714
反応ノート
読み込み中…