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Acetone → (S)-tert-butyl (1-(7-fluoro-2-(2-(methylsulfonyl)phenyl)quinolin-3-yl)-ethyl)carbamate

HRID 1019798
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HRID 1019798 반응식
[F:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[C:7]([C@@H:20]([NH:22][C:23](=[O:29])[O:24][C:25]([CH3:28])([CH3:27])[CH3:26])[CH3:21])[C:8]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[S:18][CH3:19])=[N:9]2)=[CH:4][CH:3]=1.CC(C)=[O:32].C[N+]1([O-])CCOCC1.[OH2:42]>O=[Os](=O)(=O)=O>[F:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[C:7]([C@@H:20]([NH:22][C:23](=[O:29])[O:24][C:25]([CH3:28])([CH3:27])[CH3:26])[CH3:21])[C:8]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[S:18]([CH3:19])(=[O:32])=[O:42])=[N:9]2)=[CH:4][CH:3]=1
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참가 물질

6

반응물 4

HCID 180AcetoneHCID 962WaterHCID 82029Methyl morpholine oxideHCID 86698501(S)-tert-butyl (1-(7-fluoro-2-(2-(methylthio)phenyl)quinolin-3-yl)ethyl)carbamate

생성물 1

HCID 57707808(S)-tert-butyl (1-(7-fluoro-2-(2-(methylsulfonyl)phenyl)quinolin-3-yl)-ethyl)carbamate수율 99%

시약·촉매·용매 1

HCID 30318
Osmium Tetroxide
촉매
2회

실험 절차

Under an N2 atmosphere, (S)-tert-butyl (1-(7-fluoro-2-(2-(methylthio)phenyl)-quinolin-3-yl)ethyl)carbamate (412 mg, 999 μmol) was dissolved in acetone (3.00 ml, 40.8 mmol) and water (3 mL), and NMO (351 mg, 3.00 mmol) was added followed by OsO4 (12.7 mg, 0.05 mmol). The reaction was allowed to stir at rt overnight. LC-MS showed the reaction not to be complete. The reaction was treated with OsO4 (12.7 mg, 0.05 mmol) again and stirred overnight. LC-MS showed only a trace of the starting reagent. The reaction was quenched by the addition of 5 mL of a saturated sodium thiosulfate solution. The reaction was diluted with EtOAc and washed with 5% Na2CO3. The organic layer was then washed with brine, dried (Na2SO4), filtered and concentrated in vacuo. The crude residue was purified eluting with 30% to 60% EtOAc in hexanes to provide a white solid (S)-tert-butyl (1-(7-fluoro-2-(2-(methylsulfonyl)phenyl)quinolin-3-yl)-ethyl)carbamate (440 mg, 99%). Mass Spectrum (ESI) m/e=445 (M+1).

후처리

  1. customthe reaction not
  2. stirringstirred overnight
  3. customThe reaction was quenched by the addition of 5 mL of a saturated sodium thiosulfate solution
  4. additionThe reaction was diluted with EtOAc
  5. washwashed with 5% Na2CO3
  6. washThe organic layer was then washed with brine
  7. dry with materialdried (Na2SO4)
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo
  10. customThe crude residue was purified
  11. washeluting with 30% to 60% EtOAc in hexanes

출처 및 근거

ORD 기록
ord-a9fd8a06456a4282a24b77e9aab34d20
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08716290B2

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