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Dimethyl Sulfoxide → HCID 54501125, 화합물

HRID 904825
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HRID 904825 반응식
[CH:1]([S:4]([N:7]1[C:11]2[CH:12]=[C:13]([C:16](=[CH:23][C:24]([OH:26])=[O:25])[C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)[CH:14]=[CH:15][C:10]=2[N:9]=[C:8]1[NH2:27])(=[O:6])=[O:5])([CH3:3])[CH3:2].[CH3:28]S(C)=O.[H-].[Na+].CI>O>[CH:1]([S:4]([N:7]1[C:11]2[CH:12]=[C:13]([C:16](=[CH:23][C:24]([O:26][CH3:28])=[O:25])[C:17]3[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=3)[CH:14]=[CH:15][C:10]=2[N:9]=[C:8]1[NH2:27])(=[O:5])=[O:6])([CH3:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 679Dimethyl SulfoxideHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 54254101HCID 54254101, 화합물

생성물 1

HCID 54501125HCID 54501125, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a stirred solution of 0.77 g. of 1-isopropylsulfonyl-2-amino-6-(α-hydroxycarbonylmethylenebenzyl)benzimidazole (from Example 17) in 10 ml. of dimethylsulfoxide containing 0.1 g. of a fifty percent suspension of sodium hydride in mineral oil was added in one portion 0.3 g. of methyl iodide. The reaction mixture was stirred at room temperature for fifteen minutes, and then was diluted by the addition of 50 ml. of water. The aqueous mixture was extracted several times with ethyl acetate. The extracts were combined, washed with water, dried, and the solvent was removed by evaporation under reduced pressure to provide 1-isopropylsulfonyl-2-amino-6-(α-methoxycarbonylmethylenebenzyl)benzimidazole as a yellow solid.

후처리

  1. additionwas diluted by the addition of 50 ml
  2. extractionThe aqueous mixture was extracted several times with ethyl acetate
  3. washwashed with water
  4. customdried
  5. customthe solvent was removed by evaporation under reduced pressure

출처 및 근거

ORD 기록
ord-de102f9bbf61456c8f46ac1006a30328
출처 데이터셋
uspto-grants-1983_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04420479

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