Ammonia → Benzenamine, 3,3'-methylenebis-

HRID 1719636

反応式

HRID 1719636 の反応式
[N+:1]([C:4]1[CH:5]=[C:6]([CH:19]=[CH:20][C:21]=1Cl)[C:7]([C:9]1[CH:14]=[CH:13][C:12](Cl)=[C:11]([N+:16]([O-])=O)[CH:10]=1)=O)([O-])=O.[H][H].N>[Pd].C(O)C>[CH:13]1[CH:12]=[C:11]([NH2:16])[CH:10]=[C:9]([CH2:7][C:6]2[CH:19]=[CH:20][CH:21]=[C:4]([NH2:1])[CH:5]=2)[CH:14]=1

参加物

6

反応物 3

HCID 222AmmoniaHCID 3483014,4'-Dichloro-3,3'-dinitrobenzophenoneHCID 178418361HCID 178418361、化合物2 回

生成物 1

HCID 146486Benzenamine, 3,3'-methylenebis-収率 85%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

34.1 g (0.1 mol) of 3,3'-dinitro-4,4'-dichlorbenzophenone, 1.5 g of 5% Pd/C, and 100 ml of ethanol were charged in a closed glass vessel equipped with a thermometer and a stirrer. While stirring the mixture at a temperature of 50° to 60° C., hydrogen was introduced thereinto and 22.9 l (1.02 mol) of hydrogen was absorbed in 7.5 hours. Since no more absorption of hydrogen was observed, the reaction was terminated at this point. The reaction solution was neutralized with 13.4 g (0.22 mol) of 28% aqueous ammonia and filtered to remove the catalyst. The filtrate was concentrated to give 3,3'-diaminodiphenylmethane as a brown oil. A high performance liquid chromatography revealed that the purity was 93.8%.

後処理

  1. customequipped with a thermometer and a stirrer
  2. additionwas introduced
  3. customSince no more absorption of hydrogen
  4. customthe reaction was terminated at this point
  5. filtrationfiltered
  6. customto remove the catalyst
  7. concentrationThe filtrate was concentrated

出典と根拠

ORDレコード
ord-f4816608550245f69547883a4064a4b6
出典データセット
uspto-grants-1985_09
特許番号
US04540818

関連ノート

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