Thionyl Chloride → HCID 21890740、化合物
反応式
S(Cl)(Cl)=O.O(C(CC)C(O)=O)C1C=CC=CC=1.O(C(CC)C(Cl)=O)C1C=CC=CC=1.[O:31]([CH:38]([CH2:44][CH3:45])[C:39]([N:41]=[C:42]=[S:43])=[O:40])[C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1.[Cl:46][C:47]1[CH:48]=[C:49]([CH:51]=[CH:52][C:53]=1[O:54][C:55]1[C:64]2[C:59](=[CH:60][C:61]([O:67][CH3:68])=[C:62]([O:65][CH3:66])[CH:63]=2)[N:58]=[CH:57][CH:56]=1)[NH2:50]>C(O)C.C1(C)C=CC=CC=1>[Cl:46][C:47]1[CH:48]=[C:49]([NH:50][C:42]([NH:41][C:39](=[O:40])[CH:38]([O:31][C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[CH2:44][CH3:45])=[S:43])[CH:51]=[CH:52][C:53]=1[O:54][C:55]1[C:64]2[C:59](=[CH:60][C:61]([O:67][CH3:68])=[C:62]([O:65][CH3:66])[CH:63]=2)[N:58]=[CH:57][CH:56]=1参加物
反応条件
- 温度
- 100 °C
実験手順
Toluene (20 ml) and thionyl chloride (1 ml) were added to commercially available 2-phenoxybutanoic acid (80 mg), and the mixture was heated at 100° C. for one hr. The solvent was removed by distillation, and 2-phenoxybutanoyl isothiocyanate was prepared using the resultant 2-phenoxybutanoyl chloride as a starting compound according to the description of the literature. 2-Phenoxybutanoyl isothiocyanate thus obatined was dissolved in ethanol (1 ml) to prepare a solution. 3-Chloro-4-[(6,7-dimethoxy-4-quinolyl)oxy]aniline (50 mg), toluene (5 ml), and ethanol (1 ml) were added to the solution, and the mixture was stirred at room temperature for 16 hr. The reaction solution was concentrated, and the residue was purified by chromatography on silica gel using chloroform/acetone for development to give the title compound (25 mg, yield 27%).
後処理
- customThe solvent was removed by distillation, and 2-phenoxybutanoyl isothiocyanate
- customwas prepared
- customto prepare a solution
- concentrationThe reaction solution was concentrated
- customthe residue was purified by chromatography on silica gel
出典と根拠
- ORDレコード
- ord-119b117dbd754e4f90a9320236093da7
- 出典データセット
- uspto-grants-2006_11
- 特許番号
- US07135466B2
反応ノート
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