Methane → 3-(3-Phenylpropyl)aniline

HRID 905148

反応式

HRID 905148 の反応式
[C:1]1([C:7](=O)[CH:8]=[CH:9][C:10]2[CH:15]=[CH:14][CH:13]=[C:12]([N+:16]([O-])=O)[CH:11]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.S(=O)(=O)(O)O.C.[H][H]>C(O)(=O)C.[Pd]>[C:1]1([CH2:7][CH2:8][CH2:9][C:10]2[CH:11]=[C:12]([CH:13]=[CH:14][CH:15]=2)[NH2:16])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

7

反応物 4

HCID 297MethaneHCID 1118Sulfuric AcidHCID 948623-NitrochalconeHCID 178418361HCID 178418361、化合物2 回

生成物 1

HCID 4273073-(3-Phenylpropyl)aniline収率 71.1%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 176Acetic Acid溶媒

実験手順

253 g of 1-phenyl-3-(3'-nitrophenyl)-prop-2-en-1-one are suspended in 2.5 liters of glacial acetic acid. 196 g of concentrated sulfuric acid and 10 g of 10% strength Pd on animal charcoal are added and the mixture is hydrogenated under 1.1 bar hydrogen pressure at 65°-70° C., until no further hydrogen is absorbed. When the mixture has cooled, some of the acetic acid is distilled off, the residue is rendered alkaline with sodium hydroxide solution and extracted by shaking with ether, the organic phase is dried over sodium sulfate and filtered, the solvent is stripped off and the residue is distilled. 150 g of 3-(3-phenylpropyl)-aniline of boiling point 148° C./0.2 mbar are obtained.

後処理

  1. customis absorbed
  2. temperatureWhen the mixture has cooled
  3. distillationsome of the acetic acid is distilled off
  4. extractionextracted
  5. dry with materialthe organic phase is dried over sodium sulfate
  6. filtrationfiltered
  7. distillationthe residue is distilled

出典と根拠

ORDレコード
ord-118962f8141344bbbecf904263d15b7f
出典データセット
uspto-grants-1983_12
特許番号
US04422871

関連ノート

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