Ammonia → Benzenamine, 3,3'-methylenebis-

HRID 1719636

반응식

HRID 1719636 반응식
[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

참가 물질

6

반응물 3

HCID 222AmmoniaHCID 3483014,4'-Dichloro-3,3'-dinitrobenzophenoneHCID 178418361HCID 178418361, 화합물2회

생성물 1

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

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-f4816608550245f69547883a4064a4b6
출처 데이터셋
uspto-grants-1985_09
특허 번호
US04540818

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