Benzimidazole → 1H-Benzimidazole, 1-methyl-

HRID 26699

反応式

HRID 26699 の反応式
[CH3:1]I.[OH-].[K+].[N:5]1[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=2[NH:7][CH:6]=1>C(O)C.O>[CH3:1][N:5]1[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=2[N:7]=[CH:6]1

参加物

6

反応物 3

HCID 5798BenzimidazoleHCID 6328Methyl iodideHCID 14797Potassium Hydroxide

生成物 1

HCID 958901H-Benzimidazole, 1-methyl-

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

14.1 g of methyl iodide and 6.15 g of potassium hydroxide were added to a suspension of 11.8 g of benzimidazole in 50 ml of ethanol and 30 ml of water and the mixture was refluxed for 6 hours and was then cooled. The mixture was extracted three times with chloroform and the combined chloroform extracts were dried and filtered. The filtrate was evaporated to dryness and the oily residue was chromatographed over neutral alumina. Elution with chloroform yielded 1-methyl-benzimidazole as a crude oil which was used as is for the next step.

後処理

  1. temperaturethe mixture was refluxed for 6 hours
  2. temperaturewas then cooled
  3. extractionThe mixture was extracted three times with chloroform
  4. dry with materialthe combined chloroform extracts were dried
  5. filtrationfiltered
  6. customThe filtrate was evaporated to dryness
  7. customthe oily residue was chromatographed over neutral alumina
  8. washElution with chloroform

出典と根拠

ORDレコード
ord-d0da4f3d7c0e4e4b8179c663b488848e
出典データセット
uspto-grants-1979_04
特許番号
US04151280

関連ノート

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