Bifonazole → 1,3-Bis-[alpha-(-biphenylyl)-benzyl]-imidazolium chloride

HRID 1389057

반응식

HRID 1389057 반응식
[C:1]1(C2C=CC=CC=2)[CH:6]=[CH:5][C:4]([CH:7]([N:14]2[CH:18]=[CH:17][N:16]=[CH:15]2)[C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[CH:3][CH:2]=1.[C:25]1([C:39]2[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=2)[CH:30]=[CH:29][CH:28]=[CH:27][C:26]=1[CH:31]([Cl:38])[C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1>C(#N)C>[Cl-:38].[C:25]1([C:39]2[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=2)[CH:30]=[CH:29][CH:28]=[CH:27][C:26]=1[CH:31]([N+:16]1[CH:17]=[CH:18][N:14]([CH:7]([C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:13]=2[C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[C:4]2[CH:5]=[CH:6][CH:1]=[CH:2][CH:3]=2)[CH:15]=1)[C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1

참가 물질

4

반응물 2

HCID 2378BifonazoleHCID 13823625alpha-Biphenylyl-benzyl chloride

생성물 1

HCID 202982001,3-Bis-[alpha-(-biphenylyl)-benzyl]-imidazolium chloride수율 122.2%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

31 g (0.1 mol) of 1-[α-(4-biphenylyl)-benzyl]-imidazole and 27.9 g (0.1 mol) of α-biphenylyl-benzyl chloride are suspended in 200 ml of acetonitrile. The mixture is heated under reflux for 18 hours. The reaction mixture is then concentrated by distilling off the solvent and the residue, in 500 ml of toluene, is heated under reflux. The gel thereby formed is separated off and caused to crystallise by trituration with diisopropyl ether. 36 g (62% of theory) of 1,3-bis-[α-(-biphenylyl)-benzyl]-imidazolium chloride of melting point 150° C. (with decomposition) are obtained.

후처리

  1. temperatureThe mixture is heated
  2. temperatureunder reflux for 18 hours
  3. concentrationThe reaction mixture is then concentrated
  4. distillationby distilling off the solvent
  5. temperaturethe residue, in 500 ml of toluene, is heated
  6. temperatureunder reflux
  7. customThe gel thereby formed
  8. customis separated off
  9. customto crystallise by trituration with diisopropyl ether

출처 및 근거

ORD 기록
ord-b2e8f8b42a1d4840979c37d9bd326313
출처 데이터셋
uspto-grants-1981_01
특허 번호
US04243670

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