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Oxalic Acid → N-[4-(1,3-benzodioxol-5-yl)-1-(2-hydroxyethyl)-5-methoxy-1H-pyrazol-3-yl]-2-phenyl-1-ethanesulfonamide

HRID 1368623
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1368623
C([O:4][CH2:5][CH2:6][N:7]1[C:11]([O:12][CH3:13])=[C:10]([C:14]2[CH:22]=[CH:21][C:17]3[O:18][CH2:19][O:20][C:16]=3[CH:15]=2)[C:9]([N:23](COC)[S:24]([CH2:27][CH2:28][C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)(=[O:26])=[O:25])=[N:8]1)(=O)C.C(O)(=O)C(O)=O>O.CO>[O:18]1[C:17]2[CH:21]=[CH:22][C:14]([C:10]3[C:9]([NH:23][S:24]([CH2:27][CH2:28][C:29]4[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=4)(=[O:26])=[O:25])=[N:8][N:7]([CH2:6][CH2:5][OH:4])[C:11]=3[O:12][CH3:13])=[CH:15][C:16]=2[O:20][CH2:19]1
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Komponenten

5

Edukt 2

HCID 971Oxalic AcidHCID 222819772-{4-(1,3-benzodioxol-5-yl)-5-methoxy-3-[(methoxymethyl)(phenethylsulfonyl)amino]-1H-pyrazol-1-yl}ethyl Acetate

Produkt 1

HCID 22281887N-[4-(1,3-benzodioxol-5-yl)-1-(2-hydroxyethyl)-5-methoxy-1H-pyrazol-3-yl]-2-phenyl-1-ethanesulfonamideAusbeute 54,5 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittel
HCID 962
Water
Lösungsmittel
2×

Versuchsvorschrift

2-{4-(1,3-Benzodioxol-5-yl)-5-methoxy-3-[(methoxymethyl)(phenethylsulfonyl)amino]-1H-pyrazol-1-yl}ethyl acetate (Preparation 54) (70 mg), oxalic acid (200 mg) were dissolved in a mixture of water (2 ml) and methanol (2 ml) and refluxed for two days. The reaction was diluted with water (10 ml) and the mixture was then extracted with dichloromethane (3×8 ml). The combined organic fractions were dried over sodium sulfate, concentrated under reduced pressure to yield a pale yellow oil which was purified by column chromatography (Sep-Pak™, 10 g) eluted with dichloromethane:methanol (97:3) to yield the title compound as a colourless oil (32 mg).

Aufarbeitung

  1. temperaturerefluxed for two days
  2. extractionthe mixture was then extracted with dichloromethane (3×8 ml)
  3. dry with materialThe combined organic fractions were dried over sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customto yield a pale yellow oil which
  6. customwas purified by column chromatography (Sep-Pak™, 10 g)
  7. washeluted with dichloromethane:methanol (97:3)

Quellen und Nachweise

ORD-Eintrag
ord-a447a0e91fcc4f46b0bbd65a6fab325b
Quelldatensatz
uspto-grants-2003_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06573270B1

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