2-Phenylbenzimidazole → 1-Methyl-2-phenylbenzimidazole

HRID 1358702

反応式

HRID 1358702 の反応式
[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

参加物

3

反応物 2

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

生成物 1

HCID 758071-Methyl-2-phenylbenzimidazole

反応条件

温度
90 °C

実験手順

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-phenylbenzimidazole as determined by HPLC analysis was 98%.

後処理

  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

出典と根拠

ORDレコード
ord-c498807fa1ea4e88ac9ab9ba21af462a
出典データセット
uspto-grants-2003_07
特許番号
US06596877B2

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