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1,3-Dichloro-5,5-dimethylhydantoin → Perfluorophenyl 1-(5-bromo-2-methoxyphenyl)-2-oxo-1,2-dihydroquinoline-6-sulfonate

HRID 1504438
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HRID 1504438 반응식
C(S[C:9]1[CH:10]=[C:11]2[C:16](=[CH:17][CH:18]=1)[N:15]([C:19]1[CH:24]=[C:23]([Br:25])[CH:22]=[CH:21][C:20]=1[O:26][CH3:27])[C:14](=[O:28])[CH:13]=[CH:12]2)C1C=CC=CC=1.ClN1C(C)(C)C(=O)N(Cl)C1=O.[S:40](Cl)(Cl)(=[O:42])=[O:41].[F:45][C:46]1[C:51]([F:52])=[C:50]([F:53])[C:49]([F:54])=[C:48]([F:55])[C:47]=1[OH:56]>CC#N.CC(O)=O.O>[Br:25][C:23]1[CH:22]=[CH:21][C:20]([O:26][CH3:27])=[C:19]([N:15]2[C:16]3[C:11](=[CH:10][C:9]([S:40]([O:56][C:47]4[C:46]([F:45])=[C:51]([F:52])[C:50]([F:53])=[C:49]([F:54])[C:48]=4[F:55])(=[O:42])=[O:41])=[CH:18][CH:17]=3)[CH:12]=[CH:13][C:14]2=[O:28])[CH:24]=1
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참가 물질

8

반응물 4

HCID 83601,3-Dichloro-5,5-dimethylhydantoinHCID 13041PentafluorophenolHCID 24648Sulfuryl chlorideHCID 1177369896-(benzylthio)-1-(5-bromo-2-methoxyphenyl)quinolin-2(1H)-one

생성물 1

HCID 117736973Perfluorophenyl 1-(5-bromo-2-methoxyphenyl)-2-oxo-1,2-dihydroquinoline-6-sulfonate수율 85%

시약·촉매·용매 3

HCID 176Acetic Acid용매
HCID 962Water용매2회
HCID 6342Acetonitrile용매

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온도
0 °C

실험 절차

6-(Benzylthio)-1-(5-bromo-2-methoxyphenyl)quinolin-2(1H)-one (5.48 g, 12.11 mmol) was diluted with MeCN (38.0 ml), AcOH (1.444 ml) and water (0.950 ml), and the mixture was cooled to 0° C. 1,3-Dichloro-5,5-dimethylimidazolidine-2,4-dione (3.58 g, 18.17 mmol) was added in portions and the reaction was stirred in the ice bath for 5 minutes until complete conversion to the sulfonyl chloride (reaction went from heterogeneous yellow mixture to yellow solution upon addition). With the solution at 0° C., 2,3,4,5,6-pentafluorophenol (2.68 g, 14.54 mmol) was added, followed by TEA (6.75 ml, 48.5 mmol), and the reaction was allowed to warm to RT for 20 min. Water was added and the organics were extracted with DCM (×3), followed by drying via phase separator. The organics were then concentrated in vacuo and purified via MPLC eluting with 0-100% ethyl acetate in heptanes (with 10% DCM additive) to yield perfluorophenyl 1-(5-bromo-2-methoxyphenyl)-2-oxo-1,2-dihydroquinoline-6-sulfonate (5.92 g, 10.27 mmol, 85% yield) as a white solid. MS (ESI, pos. ion) m/z: [M+1] 576.0

후처리

  1. temperatureto warm to RT for 20 min
  2. extractionthe organics were extracted with DCM (×3)
  3. customby drying via phase separator
  4. concentrationThe organics were then concentrated in vacuo
  5. custompurified via MPLC
  6. washeluting with 0-100% ethyl acetate in heptanes (with 10% DCM additive)

출처 및 근거

ORD 기록
ord-00ecb627abc941f6b4bd4f7ddc7d166b
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09212182B2

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