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Sodium Bisulfate → S-methyl--N--[4-(phenoxy)benzenesulfonyl]-D-penicillamine

HRID 1602983
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HRID 1602983 반응식
C[O:2][C:3](=[O:27])[C@@H:4]([C:22]([S:25][CH3:26])([CH3:24])[CH3:23])[NH:5][S:6]([C:9]1[CH:14]=[CH:13][C:12]([O:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)=[CH:11][CH:10]=1)(=[O:8])=[O:7].C[S-].[Na+].S(=O)(=O)(O)[O-].[Na+]>CS(C)=O>[CH3:26][S:25][C:22]([CH3:24])([CH3:23])[C@H:4]([C:3]([OH:27])=[O:2])[NH:5][S:6]([C:9]1[CH:10]=[CH:11][C:12]([O:15][C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=2)=[CH:13][CH:14]=1)(=[O:7])=[O:8]
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참가 물질

5

반응물 3

HCID 516919Sodium BisulfateHCID 4378561Sodium methanethiolateHCID 57188101S-methyl--N--[4-(phenoxy)benzenesulfonyl]-D-penicillamine methyl ester

생성물 1

HCID 56999283S-methyl--N--[4-(phenoxy)benzenesulfonyl]-D-penicillamine수율 95%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

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온도
45 °C

실험 절차

To a solution of S-methyl--N--[4-(phenoxy)benzenesulfonyl]-D-penicillamine methyl ester (0.250 g., 0.610 mmol) in DMSO (3 mL) at room temperature was added sodium thiomethoxide (171 mg., 2.44 mmol) in one portion. The solution was heated at 45° C. for18 hours, and then cooled to 0° C. and acidified to pH=5 using 1N aqueous sodium bisulfate. The mixture was partitioned between ethyl acetate and water, and the organic phase was washed with brine, dried over MgSO4, and concentrated. The residue was purified on silica eluting with 8 to 12% methanol in dichloromethane to give S-methyl--N--[4-(phenoxy)benzenesulfonyl]-D-penicillamine as a white solid in 95% yield: mp 156-158° C.; 1H--NMR (DMSO-d6) δ 1.28 (s, 3H), 1.31 (s, 3H), 1.97 (s,3H), 7.08-7.82 (m, 10H).

후처리

  1. temperaturecooled to 0° C.
  2. customThe mixture was partitioned between ethyl acetate and water
  3. washthe organic phase was washed with brine
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated
  6. customThe residue was purified on silica eluting with 8 to 12% methanol in dichloromethane

출처 및 근거

ORD 기록
ord-cef2495fb0004b9ebf6973f449b780ef
출처 데이터셋
uspto-grants-1999_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05985900

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