Ammonia → (4'-Dimethylamino phenyl]-3-ureido benzoquinoneimine

HRID 1413039

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HRID 1413039 반응식
[NH:1]([C:5]1[CH:6]=[C:7]([OH:11])[CH:8]=[CH:9][CH:10]=1)[C:2]([NH2:4])=[O:3].[NH3:12].C1(N)C(F)=C(F)C(F)=C(N)C=1F.Cl.Cl.[CH3:27][N:28]([CH3:36])[C:29]1[CH:34]=[CH:33][C:32](N)=[CH:31][CH:30]=1.S(OOS([O-])(=O)=O)([O-])(=O)=O.[NH4+].[NH4+].[OH2:49]>C(O)(C)C>[CH3:27][N:28]([CH3:36])[C:29]1[CH:34]=[CH:33][C:32]([C:9]2[C:10](=[O:49])[CH:5]([NH:1][C:2]([NH2:4])=[O:3])[C:6](=[NH:12])[C:7](=[O:11])[CH:8]=2)=[CH:31][CH:30]=1

참가 물질

8

반응물 6

HCID 222AmmoniaHCID 962Water2회HCID 7472N,N-dimethyl-p-phenylenediamineHCID 12796m-HydroxyphenylureaHCID 62648Ammonium PersulfateHCID 149026Tetrafluoro-m-phenylenediamine dihydrochloride

생성물 1

HCID 131710439(4'-Dimethylamino phenyl]-3-ureido benzoquinoneimine

시약·촉매·용매 1

HCID 3776Isopropanol용매

반응 조건

온도
0 °C

실험 절차

0.03 mole (4.56 g) of 3-ureido phenol is dissolved in 100 cc of isopropyl alcohol to which have been added 100 cc of ammonia at 22° Be. 350 g of crushed ice are then added to this solution. The resulting reaction mixture is maintained at about 0° C., and there are introduced simultaneously, with good agitation and with the aid of a double funnel, 0.03 mole (6.27 g) of the dihydrochloride of N,N-dimethyl paraphenylenediamine in 50 cc of water and 0.060 mole (13.7 g) of ammonium persulfate in 50 cc of water. At the end of this addition, the agitation is continued for 15 minutes and the above indoaniline which has precipitated is then filtered, washed with water, recrystallized in a mixture of dimethylformamide in water and dried under a vacuum. It exhibits a melting point of 226° C.

후처리

  1. customThe resulting reaction mixture
  2. additionthere are introduced simultaneously, with good agitation and with the aid of a double funnel
  3. additionAt the end of this addition
  4. customthe above indoaniline which has precipitated
  5. filtrationis then filtered
  6. washwashed with water
  7. customrecrystallized in a mixture of dimethylformamide in water
  8. customdried under a vacuum

출처 및 근거

ORD 기록
ord-4a7cea257bc9420e9612f16fff1bd406
출처 데이터셋
uspto-grants-1981_02
특허 번호
US04248591

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