Monoperoxyphthalic Acid Magnesium Salt → 8-{3-[1-(4-Chloro-phenyl)-2-(1-oxy-pyridin-4-yl)-ethyl]-phenyl}-6-isopropyl-quinoline

HRID 896685Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 896685
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:16]2[CH:17]=[C:18]([C:22]3[CH:23]=[C:24]([CH:32]([CH3:34])[CH3:33])[CH:25]=[C:26]4[C:31]=3[N:30]=[CH:29][CH:28]=[CH:27]4)[CH:19]=[CH:20][CH:21]=2)[CH2:9][C:10]2[CH:15]=[CH:14][N:13]=[CH:12][CH:11]=2)=[CH:4][CH:3]=1.C1C=C(C([O-])=[O:42])C(C(O[O-])=O)=CC=1.[Mg+2]>C(Cl)Cl.CO.C(=O)(O)[O-].[Na+].C(OCC)(=O)C>[CH3:33][CH:32]([C:24]1[CH:25]=[C:26]2[CH:27]=[CH:28][CH:29]=[N:30][C:31]2=[C:22]([C:18]2[CH:19]=[CH:20][CH:21]=[C:16]([CH:8]([C:5]3[CH:6]=[CH:7][C:2]([Cl:1])=[CH:3][CH:4]=3)[CH2:9][C:10]3[CH:11]=[CH:12][N+:13]([O-:42])=[CH:14][CH:15]=3)[CH:17]=2)[CH:23]=1)[CH3:34]

Komponenten

6

Edukt 2

HCID 10130449Monoperoxyphthalic Acid Magnesium SaltHCID 101831968-(3-(1-(4-Chlorophenyl)-2-(pyridin-4-yl)ethyl)phenyl)-6-isopropylquinoline

Produkt 1

HCID 102059788-{3-[1-(4-Chloro-phenyl)-2-(1-oxy-pyridin-4-yl)-ethyl]-phenyl}-6-isopropyl-quinoline

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 8857Ethyl AcetateLösungsmittelHCID 516892Sodium BicarbonateLösungsmittelHCID 21226129Dichloromethane methanolLösungsmittel

Versuchsvorschrift

To a solution of Example 60 (100 mg, 0.22 mmol) in CH2Cl2/MeOH (1:1, 6 mL) was added MMPP (320 mg, 0.65 mmol). After 18 h, the resulting reaction mixture was diluted with a sodium bicarbonate solution and ethyl acetate. The organic extracts were washed (H2O, brine), dried (MgSO4), filtered and concentrated. Purification by flash chromatography (eluting with ethanol/ethyl acetate, 10:90 to 25:75) provided the title compound.

Aufarbeitung

  1. customthe resulting reaction mixture
  2. washThe organic extracts were washed (H2O, brine)
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customPurification
  7. washby flash chromatography (eluting with ethanol/ethyl acetate, 10:90 to 25:75)

Quellen und Nachweise

ORD-Eintrag
ord-c0af372188c1414f9ec337d53316ca98
Quelldatensatz
uspto-grants-2005_07
Patentnummer
US06919353B2

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