HCID 21472721, Verbindung → HCID 69945089, Verbindung

HRID 1736474Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1736474
C(OC([N:8]1[C:12]2[C:13]([F:25])=[CH:14][C:15]([NH:18]C(NCCN)=S)=[C:16]([CH3:17])[C:11]=2[N:10]=[CH:9]1)=O)(C)(C)C>CO>[F:25][C:13]1[C:12]2[N:8]=[CH:9][NH:10][C:11]=2[C:16]([CH3:17])=[C:15]([NH:18][N:10]2[CH2:11][CH2:12][N:8]=[CH:9]2)[CH:14]=1

Komponenten

3

Edukt 1

HCID 21472721HCID 21472721, Verbindung

Produkt 1

HCID 69945089HCID 69945089, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

A mixture of N-(1-tert-butoxycarbonyl-7-fluoro-4-methyl-5-benzimidazolyl)-N'-2-aminoethylthio-urea (0.5 g) and mercuric acetate (0.52 g) in methanol (150 mL) is stirred at room temperature for 1 hour. The resulting black mixture is filtered on Celite with methanol wash of the solids. The filtrate is rotary evaporated and the residue filtered through a short pad of silica gel, eluting 25% methanol in chloroform containing 1% of ammonium hydroxide. The product-containing fractions are rotary evaporated, the residue diluted with water (15 mL), filtered through a plug of glass wool and lyophilized to afford 7-fluoro-4-methyl-5-(2-imidazolinylamino)benzimidazole as a pale yellow solid.

Aufarbeitung

  1. filtrationThe resulting black mixture is filtered on Celite with methanol
  2. washwash of the solids
  3. customThe filtrate is rotary evaporated
  4. filtrationthe residue filtered through a short pad of silica gel
  5. washeluting 25% methanol in chloroform containing 1% of ammonium hydroxide
  6. additionthe residue diluted with water (15 mL)
  7. filtrationfiltered through a plug of glass wool

Quellen und Nachweise

ORD-Eintrag
ord-a5a8efc387c140f2b2884fef9e5f5955
Quelldatensatz
uspto-grants-1996_07
Patentnummer
US05541210

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