Hydrochloric Acid → 4,5-Diamino-2',7'-difluoro-3',6'-dihydroxy-spiro[isobenzofuran-1(3H),9'-[9H]-xanthen]-3-one

HRID 2307886Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2307886
[NH2:1][C:2]1[C:27]([N+:28]([O-])=O)=[CH:26][CH:25]=[C:24]2[C:3]=1[C:4](=[O:31])[O:5][C:6]12[C:19]2[CH:18]=[C:17]([F:20])[C:16]([OH:21])=[CH:15][C:14]=2[O:13][C:12]2[C:7]1=[CH:8][C:9]([F:23])=[C:10]([OH:22])[CH:11]=2.Cl>>[NH2:1][C:2]1[C:27]([NH2:28])=[CH:26][CH:25]=[C:24]2[C:3]=1[C:4](=[O:31])[O:5][C:6]12[C:7]2[CH:8]=[C:9]([F:23])[C:10]([OH:22])=[CH:11][C:12]=2[O:13][C:14]2[C:19]1=[CH:18][C:17]([F:20])=[C:16]([OH:21])[CH:15]=2

Komponenten

3

Edukt 2

HCID 313Hydrochloric AcidHCID 130077224-Amino-5-nitro-2',7'-difluoro-3',6'-dihydroxy-spiro [isobenzofuran-1(3h),9'-[9h]xanthen]-3-one

Produkt 1

HCID 130077234,5-Diamino-2',7'-difluoro-3',6'-dihydroxy-spiro[isobenzofuran-1(3H),9'-[9H]-xanthen]-3-oneAusbeute 78,7 %

Versuchsvorschrift

4-Amino-5 -nitro-2′,7′-difluoro-3′,6′-dihydroxy-spiro [isobenzofuran-1(3H),9′-[9H]xanthen]-3-one (1.3 g, 3.0 mmol) was added to an aqueous solution of Na2S and NaSH, and the mixture was refluxed for 24 hours. The reaction mixture was cooled, and adjusted to pH 3 with hydrochloric acid, and precipitates were collected by filtration. The obtained product was dried and purified by silica gel chromatography to obtain the title compound (0.94 g, 78%).

Aufarbeitung

  1. temperaturethe mixture was refluxed for 24 hours
  2. temperatureThe reaction mixture was cooled
  3. customprecipitates
  4. filtrationwere collected by filtration
  5. customThe obtained product was dried
  6. custompurified by silica gel chromatography

Quellen und Nachweise

ORD-Eintrag
ord-44a334692cc748188a5f140c3672c7cc
Quelldatensatz
uspto-grants-2004_12
Patentnummer
US06833386B2

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