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1,1'-Carbonyldiimidazole → HCID 22663495, 화합물

HRID 392641
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HRID 392641 반응식
C(N1C=CN=C1)(N1C=CN=C1)=O.[CH3:13][C:14]1[CH:19]=[CH:18][C:17]([S:20]([O:23][CH2:24][C@@H:25]2[O:30][C:29]3[C:31]([OH:40])=[C:32]([NH:35][C:36]([O:38]C)=O)[CH:33]=[CH:34][C:28]=3[O:27][CH2:26]2)(=[O:22])=[O:21])=[CH:16][CH:15]=1>C(Cl)Cl>[CH3:13][C:14]1[CH:15]=[CH:16][C:17]([S:20]([O:23][CH2:24][CH:25]2[CH2:26][O:27][C:28]3[CH:34]=[CH:33][C:32]4[NH:35][C:36](=[O:38])[O:40][C:31]=4[C:29]=3[O:30]2)(=[O:22])=[O:21])=[CH:18][CH:19]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 682631,1'-CarbonyldiimidazoleHCID 86587694HCID 86587694, 화합물

생성물 1

HCID 22663495HCID 22663495, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

1,1′-Carbonyldiimidazole (6.45 g, 39.6 mmole) was added to a solution of {(2R)-8-hydroxy-7-[(methoxycarbonyl)amino]-2,3-dihydro-1,4-benzodioxin-2-yl}-methyl 4-methylbenzenesulfonate (5.40 g, 13.2 mmole) in methylene chloride (400 mL), the solution was refluxed for 4 hours under nitrogen. The solvent was then removed in vacuum and was replaced with 2N aqueous HCl (150 mL). After the mixture had been stirred for 0.5 hour at room temperature, a white solid precipitate, the (R)-enantiomer of the title compound, was removed by filtration, and was dried under high vacuum (5.0 g, >99%).

후처리

  1. temperaturethe solution was refluxed for 4 hours under nitrogen
  2. customThe solvent was then removed in vacuum
  3. customa white solid precipitate, the (R)-enantiomer of the title compound, was removed by filtration
  4. customwas dried under high vacuum (5.0 g, >99%)

출처 및 근거

ORD 기록
ord-59665b144af448a68dccc15e7a071863
출처 데이터셋
uspto-grants-2004_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06800648B2

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