Methyl iodide → HCID 18979095、化合物
反応式
[Br:1][C:2]1[CH:11]=[CH:10][C:9]([O:12][CH3:13])=[C:8]2[C:3]=1[CH:4]=[CH:5][C:6]([NH:14][C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])=[N:7]2.O1CCC[CH2:23]1.[H-].[Na+].IC>C(OCC)(=O)C>[Br:1][C:2]1[CH:11]=[CH:10][C:9]([O:12][CH3:13])=[C:8]2[C:3]=1[CH:4]=[CH:5][C:6]([N:14]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH3:23])=[N:7]2参加物
6
実験手順
5-Bromo-2-t-butyloxycarbonylamino-8-Methoxyquinoline (1.21 g) and tetrahydrofuran (20 ml) were combined at room temperature under a nitrogen atmosphere. Sodium hydride (60% dispersion in oil) (164 mg) was added and the reaction mixture stirred for 2 h whilst effervescence occurred and a yellow colour appeared. Iodomethane (0.43 ml) was then added and stirring was continued for 2 h after which time the reaction was diluted with ethyl acetate (100 ml), washed successively with water, saturated aqueous sodium bicarbonate and brine, then dried (magnesium sulphate) and evaporated in vacuo to give the title compound (1.1 g) as a yellow solid.
後処理
- customwere combined at room temperature under a nitrogen atmosphere
- stirringstirring
- waitwas continued for 2 h
- washwashed successively with water, saturated aqueous sodium bicarbonate and brine
- dry with materialdried (magnesium sulphate)
- customevaporated in vacuo
出典と根拠
- ORDレコード
- ord-8da48e0f22ce4333aa4ab2cfb937ba4a
- 出典データセット
- uspto-grants-1998_09
- 特許番号
- US05804588
反応ノート
読み込み中…