Hydrochloric Acid → HCID 22225628, Verbindung

HRID 2217364Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2217364
Cl.[F:2][C:3]1[C:11]([F:12])=[C:10]2[C:6]([C:7]([NH2:21])=[N:8][N:9]2COCC[Si](C)(C)C)=[CH:5][C:4]=1[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1>CO>[F:2][C:3]1[C:11]([F:12])=[C:10]2[C:6]([C:7]([NH2:21])=[N:8][NH:9]2)=[CH:5][C:4]=1[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 9976768HCID 9976768, Verbindung

Produkt 1

HCID 22225628HCID 22225628, VerbindungAusbeute 72,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

1.1 ml of 2N HCl are added to 661 mg of 6,7-difluoro-5-phenyl-1-[[2-(trimethylsilyl)ethoxy]methyl]-1H-indazole-3-amine in 15 ml of methanol. The reaction is subjected to microwaves for 3 minutes at 140° C. After hydrolysis with saturated KH2PO4 solution and extraction with methylene chloride, the solvents are evaporated off and the residue is chromatographed on silica (methylene chloride/ethyl acetate) to give 314 mg of 6,7-difluoro-5-phenyl-1H-indazole-3-amine.

Aufarbeitung

  1. customAfter hydrolysis
  2. extractionwith saturated KH2PO4 solution and extraction with methylene chloride
  3. customthe solvents are evaporated off
  4. customthe residue is chromatographed on silica (methylene chloride/ethyl acetate)

Quellen und Nachweise

ORD-Eintrag
ord-5f76ec9a087d42a4b3934fcb1021db99
Quelldatensatz
uspto-grants-2008_08
Patentnummer
US07407981B2

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