反応式
Cl[C:2]1[C:11]2[C:6](=[C:7]([O:14][CH3:15])[CH:8]=[CH:9][C:10]=2[O:12][CH3:13])[N:5]=[CH:4][C:3]=1[C:16]#[N:17].Cl.Cl.[CH3:20][N:21]([CH3:29])[C:22]1[CH:27]=[CH:26][CH:25]=[C:24]([NH2:28])[CH:23]=1.C(OC(O)C)C>N1C=CC=CC=1>[CH3:20][N:21]([CH3:29])[C:22]1[CH:23]=[C:24]([NH:28][C:2]2[C:11]3[C:6](=[C:7]([O:14][CH3:15])[CH:8]=[CH:9][C:10]=3[O:12][CH3:13])[N:5]=[CH:4][C:3]=2[C:16]#[N:17])[CH:25]=[CH:26][CH:27]=1参加物
5
実験手順
A mixture of 0.148 g of 4-chloro-5,8-dimethoxy-3-quinolinecarbonitrile, 0.146 g of N,N-dimethyl-1,3-phenylenediamine dihydrochloride, 0.2 ml of pyridine, and 5 ml of ethoxyethanol was stirred under nitrogen, at reflux temperature for 30 minutes. Then the mixture was partitioned between ethyl acetate and saturated sodium chloride solution. The organic layer was dried and concentrated in vacuo. The residue thus obtained was chromatographed on silica gel eluting with ethyl acetate. Solvent was removed from product fractions giving 0.160 g of 4-(3-dimethylamino-phenylamino)-5,8-dimethoxy-quinoline-3-carbonitrile as a solid, mp 103-105° C.; mass spectrum (EI, m/e): M 348.1588.
後処理
- temperatureat reflux temperature for 30 minutes
- customThen the mixture was partitioned between ethyl acetate and saturated sodium chloride solution
- customThe organic layer was dried
- concentrationconcentrated in vacuo
- customThe residue thus obtained
- customwas chromatographed on silica gel eluting with ethyl acetate
- customSolvent was removed from product fractions
出典と根拠
- ORDレコード
- ord-9a9221bcd5094dbea5d4910619fe94c9
- 出典データセット
- uspto-grants-1999_12
- 特許番号
- US06002008
関連ノート
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