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Dimethyl Sulfate → 6-Benzoyl-1-methyl-2-(2-pyridylsulfinylmethyl)benzimidazole

HRID 414191
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HRID 414191 반응식
[C:1]([C:9]1[CH:26]=[CH:25][C:12]2[N:13]=[C:14]([CH2:16][S:17]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][N:20]=3)=[O:18])[NH:15][C:11]=2[CH:10]=1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[Na+].S(OC)(O[CH3:33])(=O)=O>C(O)C.O>[C:1]([C:9]1[CH:26]=[CH:25][C:12]2[N:13]([CH3:33])[C:14]([CH2:16][S:17]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][N:20]=3)=[O:18])=[N:15][C:11]=2[CH:10]=1)(=[O:8])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1.[C:1]([C:9]1[CH:26]=[CH:25][C:12]2[N:13]=[C:14]([CH2:16][S:17]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][N:20]=3)=[O:18])[N:15]([CH3:33])[C:11]=2[CH:10]=1)(=[O:8])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 6497Dimethyl SulfateHCID 14798Sodium HydroxideHCID 139611705-Benzoyl-2-(2-pyridylsulfinylmethyl)benzimidazole

생성물 2

HCID 139611875-Benzoyl-1-methyl-2-(2-pyridylsulfinylmethyl)benzimidazole수율 12.5%HCID 139611886-Benzoyl-1-methyl-2-(2-pyridylsulfinylmethyl)benzimidazole수율 40%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

A mixture of 3.61 g of 5-benzoyl-2-(2-pyridylsulfinylmethyl)benzimidazole (0.01 mole), 0.40 g of sodium hydroxide (0.01 mole) and 2 ml of dimethyl sulfate (0.02 mole) in 50 ml of ethanol and 5 ml of water is maintained under reflux for 3 hours. The ethanol is evaporated off and the residue diluted with water and extracted with chloroform. The organic phase is washed with water, dried and evaporated. The residue is chromatographed with silica gel, using chloroform/methanol (99:1) and subsequently chloroform/methanol (95:5) as eluant. On fractional crystallization of the final fraction in ethyl acetate, 0.47 g (12.5%) of 5-benzoyl-1-methyl-2-(2-pyridylsulfinylmethyl)benzimidazole, melting point 174°-177° C., and 1.5 g (40%) of 6-benzoyl-1-methyl-2-(2-pyridylsulfinylmethyl)benzimidazole, melting point 181°-183° C., are obtained.

후처리

  1. temperatureis maintained
  2. temperatureunder reflux for 3 hours
  3. customThe ethanol is evaporated off
  4. additionthe residue diluted with water
  5. extractionextracted with chloroform
  6. washThe organic phase is washed with water
  7. customdried
  8. customevaporated
  9. customThe residue is chromatographed with silica gel
  10. customOn fractional crystallization of the final fraction in ethyl acetate

출처 및 근거

ORD 기록
ord-b6f700a299384ce38dc192de4a8234d1
출처 데이터셋
uspto-grants-1988_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04791114

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