反応式
[C:1]([CH:3]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)[C:4]([OH:6])=[O:5])#[N:2].[Cl:13][C:14]1[C:19](O)=[C:18]([Cl:21])[C:17]([Cl:22])=[C:16]([Cl:23])[C:15]=1[Cl:24].O=P(Cl)(Cl)Cl.Cl>C(Cl)(Cl)(Cl)Cl>[Cl:13][C:14]1[C:19]([O:5][C:4](=[O:6])[CH:3]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[C:1]#[N:2])=[C:18]([Cl:21])[C:17]([Cl:22])=[C:16]([Cl:23])[C:15]=1[Cl:24]参加物
6
実験手順
8 g. (0.05 moles) of α-cyanophenylacetic acid, 13 g. (0.05 moles) of pentachlorophenol are mixed together. 4.3 g. (0.05 moles) of phosphoroxychloride are added dropwise. The obtained mixture is heated slowly to 85°-90° C. on an oil-bath and the mixture is kept at this temperature until the HCl evolution ceases. When the reaction is completed, the mixture is cooled to room temperature, and the melt is taken up in 100 ml. of carbon tetrachloride. The solution is washed three times with 30 ml. of water, treated with decolorizing charcoal, dried and evaporated. The product is recrystalized from diisopropyl ether, and crystalline pentachlorophenyl ester is precipitated.
後処理
- temperatureThe obtained mixture is heated slowly to 85°-90° C. on an oil-bath
- washThe solution is washed three times with 30 ml
- additionof water, treated with decolorizing charcoal
- customdried
- customevaporated
- customThe product is recrystalized from diisopropyl ether, and crystalline pentachlorophenyl ester
- customis precipitated
出典と根拠
- ORDレコード
- ord-18a9a5d6942141388dbe7abf23f673ab
- 出典データセット
- uspto-grants-1985_04
- 特許番号
- US04508658
関連ノート
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