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Acetonitrile → 4-(4-Phenylphenyl)imidazole-1,2-diamine

HRID 357614
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인쇄 미리보기

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HRID 357614 반응식
[NH2:1][C:2]1[N:3]([N:19]=CC2C=CC=CC=2)[CH:4]=[C:5]([C:7]2[CH:12]=[CH:11][C:10]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)=[CH:9][CH:8]=2)[N:6]=1.O.NN.C(#N)C>C(O)COCCO>[NH2:19][N:3]1[CH:4]=[C:5]([C:7]2[CH:8]=[CH:9][C:10]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)=[CH:11][CH:12]=2)[N:6]=[C:2]1[NH2:1]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6342AcetonitrileHCID 24654Hydrazine hydrate (1:1)HCID 39800002-Amino-1-benzylideneamino-4-(4-biphenylyl)-imidazole

생성물 1

HCID 9150354-(4-Phenylphenyl)imidazole-1,2-diamine

시약·촉매·용매 1

HCID 8117Diethylene Glycol용매

반응 조건

온도
20 °C

실험 절차

A solution of 9.2 g (0.0189 mol) of 2-amino-1-benzylideneamino-4-(4-biphenylyl)-imidazole and 22 ml of hydrazine hydrate in 73 ml of diethylene glycol is stirred at 140° C. for 48 hours. After cooling to 20° C., 100 ml of acetonitrile are added to the reaction mixture, which is then cooled further to 5° C. The product that has separated out is filtered off and washed with acetonitrile and diethyl ether. In that manner there is obtained the title compound having a water content of 0.41 %, m.p. >280° C., 1H-NMR (DMSO): δ=7.29-7.73 (m, 9H); 7.12 (s, 1H); 5.55 (s, 2H); 5.39 (s, 2H).

후처리

  1. temperatureis then cooled further to 5° C
  2. customThe product that has separated out
  3. filtrationis filtered off
  4. washwashed with acetonitrile and diethyl ether

출처 및 근거

ORD 기록
ord-e7fa5f72c3074203b8911dfac0b85803
출처 데이터셋
uspto-grants-1998_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05840911

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