Hydrochloric Acid → HCID 21958032, Verbindung

HRID 2299222Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2299222
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[NH:9][S:10]([CH:13]1[C:18]([C:19]([O:21][CH2:22][C:23]([O:25]C(C)(C)C)=[O:24])=[O:20])=[CH:17][CH2:16][CH2:15][CH2:14]1)(=[O:12])=[O:11].Cl>C(OCC)(=O)C>[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[NH:9][S:10]([CH:13]1[C:18]([C:19]([O:21][CH2:22][C:23]([OH:25])=[O:24])=[O:20])=[CH:17][CH2:16][CH2:15][CH2:14]1)(=[O:12])=[O:11]

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 86758707HCID 86758707, Verbindung2×

Produkt 1

HCID 21958032HCID 21958032, VerbindungAusbeute 35,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel2×

Versuchsvorschrift

To a solution of t-butyl [6-[N-(2,4-difluorophenyl)sulfamoyl]-1-cyclohexen-1-yl]carbonyloxyacetate (Compound 59, 80 mg) obtained in Example 56 in ethyl acetate (4 ml), a 4N solution of hydrogen chloride in ethyl acetate (5 ml) was added with ice-cooling and the mixture was stirred at room temperature for 70 hours. The reaction mixture was evaporated under reduced pressure to dryness and the residue was purified by ODS column chromatography (eluent: methanol/water=3/2) to yield [6-[N-(2,4-difluorophenyl)sulfamoyl]-1-cyclohexen-1-yl]carbonyloxyacetic acid (Compound 60, 25 mg) as white powdery crystals.

Aufarbeitung

  1. temperaturecooling
  2. customThe reaction mixture was evaporated under reduced pressure to dryness
  3. customthe residue was purified by ODS column chromatography (eluent: methanol/water=3/2)

Quellen und Nachweise

ORD-Eintrag
ord-27e50f150c9f4092a0574635a63dc291
Quelldatensatz
uspto-grants-2002_12
Patentnummer
US06495604B1

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