反応式
Br[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][O:8][CH2:9][CH2:10][CH2:11][CH2:12][C:13]1[CH:18]=[CH:17][C:16]([N+:19]([O-:21])=[O:20])=[CH:15][CH:14]=1.[CH2:22]([NH2:29])[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1>Cl>[N+:19]([C:16]1[CH:17]=[CH:18][C:13]([CH2:12][CH2:11][CH2:10][CH2:9][O:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][NH:29][CH2:22][C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)=[CH:14][CH:15]=1)([O-:21])=[O:20]参加物
4
実験手順
1-[4-[(6-Bromohexyl)oxy]butyl]-4-nitrobenzene (8.0 g) was added dropwise to benzylamine (30 ml) at 110°. The solution was heated at 110°-120° for 2 h, treated with hydrochloric acid (2M; 200 ml), and extracted with ethyl acetate (2×150 ml). The organic extract was washed with aqueous sodium carbonate (150 ml) and brine (150 ml), dried and evaporated. The residue was purified by FCC eluting with ether to give the title compound as a pale yellow oil (5.9 g). T.l.c. Ether Rf 0.15.
後処理
- temperatureThe solution was heated at 110°-120° for 2 h
- extractionextracted with ethyl acetate (2×150 ml)
- extractionThe organic extract
- washwas washed with aqueous sodium carbonate (150 ml) and brine (150 ml)
- customdried
- customevaporated
- customThe residue was purified by FCC
- washeluting with ether
出典と根拠
- ORDレコード
- ord-b8b288a265c943239010e50fc974339e
- 出典データセット
- uspto-grants-1989_08
- 特許番号
- US04853381
関連ノート
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