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

HRID 1719638

반응식

HRID 1719638 반응식
[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

참가 물질

6

반응물 3

HCID 222AmmoniaHCID 554735(4-Chloro-3-nitrophenyl)(4-nitrophenyl)methanoneHCID 178418361HCID 178418361, 화합물2회

생성물 1

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

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 8076Glycol monoethyl ether용매

실험 절차

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%.

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

출처 및 근거

ORD 기록
ord-c5bfde3dbf194434ab83be76cf615e33
출처 데이터셋
uspto-grants-1985_09
특허 번호
US04540818

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