Ammonia → Benzenamine, 3-((4-aminophenyl)methyl)-

HRID 1719638

反応式

HRID 1719638 の反応式
[N+:1]([C:4]1[CH:5]=[C:6]([CH:18]=[CH:19][C:20]=1Cl)[C:7]([C:9]1[CH:14]=[CH:13][C:12]([N+:15]([O-])=O)=[CH:11][CH:10]=1)=O)([O-])=O.[H][H].N>[Pd].CCOCCO>[CH:19]1[CH:20]=[C:4]([NH2:1])[CH:5]=[C:6]([CH2:7][C:9]2[CH:14]=[CH:13][C:12]([NH2:15])=[CH:11][CH:10]=2)[CH:18]=1

参加物

6

反応物 3

HCID 222AmmoniaHCID 554735(4-Chloro-3-nitrophenyl)(4-nitrophenyl)methanoneHCID 178418361HCID 178418361、化合物2 回

生成物 1

HCID 146674Benzenamine, 3-((4-aminophenyl)methyl)-

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 8076Glycol monoethyl ether溶媒

実験手順

15.3 g (0.05 mol) of 3,4'-dinitro-4-chlorobenzophenone, 0.75 g of 5% Pd/C and 50 ml of ethyl cellosolve were charged in a closed glass vessel equipped with a thermometer and a stirrer. While stirring the mixture at a temperature of 75° to 80° C., hydrogen was introduced thereinto and 10.3 l (0.46 mol) of hydrogen was absorbed in 13 hours. Since no more absorption of hydrogen was observed, the reaction was terminated at this point. The reaction solution was neutralized with 3.6 g (0.06 mol) of 28% aqueous ammonia. The catalyst was removed by filtration. The filtrate was concentrated to obtain 3,4'-diaminodiphenylmethane as a brown oil. A high performance liquid chromatography revealed that the purity was 88.2%.

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. customThe catalyst was removed by filtration
  6. concentrationThe filtrate was concentrated

出典と根拠

ORDレコード
ord-c5bfde3dbf194434ab83be76cf615e33
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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