Benzyl Chloride → 1-Benzyl-2-phenyl-1H-benzoimidazole

HRID 1926470노트

반응식

HRID 1926470 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.C(=O)([O-])[O-].[K+].[K+].[CH2:22](Cl)[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1>CN(C)C=O>[CH2:22]([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)[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1

참가 물질

5

반응물 3

HCID 7503Benzyl ChlorideHCID 11430Potassium CarbonateHCID 128552-Phenylbenzimidazole

생성물 1

HCID 12216871-Benzyl-2-phenyl-1H-benzoimidazole

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a flask were added 3 g 2-phenylbenzimidazole, 2.8 g potassium carbonate, 40 ml N,N-dimethylformamide and the mixture was stirred under nitrogen. 3.6 g Benzyl chloride were added and the mixture was heated to 75 C for 8 hrs. The reaction was cooled to 50 C and quenched with 40 ml of water and cooled to 5 C. The product was filtered, washed with water. The product was recrystallized by dissolving in 57 ml acetonitrile at reflux and 39 ml water were added. After cooling to 5 C, the product was filtered, washed and dried giving 3.1 g.

후처리

  1. temperaturethe mixture was heated to 75 C for 8 hrs
  2. temperatureThe reaction was cooled to 50 C
  3. customquenched with 40 ml of water
  4. temperaturecooled to 5 C
  5. filtrationThe product was filtered
  6. washwashed with water
  7. customThe product was recrystallized
  8. dissolutionby dissolving in 57 ml acetonitrile
  9. temperatureat reflux
  10. addition39 ml water were added
  11. temperatureAfter cooling to 5 C
  12. filtrationthe product was filtered
  13. washwashed
  14. customdried
  15. customgiving 3.1 g

출처 및 근거

ORD 기록
ord-5f4c324b8b144d039973850eb1b44b7c
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08182718B2

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