Benzimidazole → 1H-Benzimidazole, 1-methyl-

HRID 26699

반응식

HRID 26699 반응식
[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

참가 물질

6

반응물 3

HCID 5798BenzimidazoleHCID 6328Methyl iodideHCID 14797Potassium Hydroxide

생성물 1

HCID 958901H-Benzimidazole, 1-methyl-

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d0da4f3d7c0e4e4b8179c663b488848e
출처 데이터셋
uspto-grants-1979_04
특허 번호
US04151280

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