2-Phenylbenzimidazole → 1-Methyl-2-phenylbenzimidazole

HRID 49692

반응식

HRID 49692 반응식
[C:1]1([C:7]2[NH:8][C:9]3[CH:15]=[CH:14][CH:13]=[CH:12][C:10]=3[N:11]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH2:16]1CCN2C(=NCCC2)CC1>>[CH3:16][N:11]1[C:10]2[CH:12]=[CH:13][CH:14]=[CH:15][C:9]=2[N:8]=[C:7]1[C:1]1[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

참가 물질

3

반응물 2

HCID 128552-PhenylbenzimidazoleHCID 811841,8-Diazabicyclo(5.4.0)undec-7-ene

생성물 1

HCID 758071-Methyl-2-phenylbenzimidazole

반응 조건

온도
90 °C

실험 절차

To a mixture of 2-phenylbenzimidazole (1.02 g, 5.25 mmol) in DMC (10 mL), DBU (0.80 g, 5.25 mmol) was added and the resulting mixture was heated to reflux (90° C.) for 6 hours. The solvent was evaporated under vacuum and the resulting oil was dissolved in methylene chloride (2 mL) and filtered through silica gel (2:1 EtOA/hexane). The solvent was evaporated under vacuum to afford 1-methyl-2-phenylbenzimidazole as a solid. The yield of 1-methyl-2-phenylbenzimiazole as determined by HPLC analysis was 98%.

후처리

  1. additionwas added
  2. temperaturethe resulting mixture was heated
  3. customThe solvent was evaporated under vacuum
  4. dissolutionthe resulting oil was dissolved in methylene chloride (2 mL)
  5. filtrationfiltered through silica gel (2:1 EtOA/hexane)
  6. customThe solvent was evaporated under vacuum

출처 및 근거

ORD 기록
ord-ff7dc106ad254b359a888c4714010314
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06706929B2

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