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Methanesulfonyl chloride → HCID 57976191, 화합물

HRID 420890
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HRID 420890 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:12](=[O:13])[C:11]([CH2:15][OH:16])([CH3:14])[NH:10][C:9]2=[O:17])=[CH:4][C:3]=1[C:18]([F:21])([F:20])[F:19].[CH3:22][S:23](Cl)(=[O:25])=[O:24]>C(Cl)Cl>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:12](=[O:13])[C:11]([CH2:15][O:16][S:23]([CH3:22])(=[O:25])=[O:24])([CH3:14])[NH:10][C:9]2=[O:17])=[CH:4][C:3]=1[C:18]([F:19])([F:21])[F:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 31297Methanesulfonyl chlorideHCID 57976187HCID 57976187, 화합물

생성물 1

HCID 57976191HCID 57976191, 화합물수율 85%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

3-(4-Chloro-3-trifluoromethyl-phenyl)-5-hydroxymethyl-5-methyl-imidazolidine-2,4-dione from Example 10 (1.01 g, 3.14 mmoL) in DCM (10 mL) was treated with TEA (0.66 mL, 4.70 mmoL) followed by MsCl (360 mg, 3.14 mmoL) at 0° C., The reaction was slowly warmed to room temperature and stirring for another 2 hrs. The crude product was partitioned between DCM and water. The organic layer was washed with sat. NaHCO3, brine, dried over anhydrous Na2SO4, filtered and concentrated, then purified by silica gel column chromatography using heptane and ethyl acetate as eluent to afford the title compound as a white solid (1.05 g, yield 85%).

후처리

  1. customThe crude product was partitioned between DCM and water
  2. washThe organic layer was washed with sat. NaHCO3, brine
  3. dry with materialdried over anhydrous Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated
  6. custompurified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-6f4a1965e2c14ffd912c2a6dfacbe06e
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08097730B2

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