Benzylamine → 6-chloro-1-hydroxy-2-(trifluoromethyl)-1H-imidazo(4,5-b)pyridine benzylamine salt

HRID 371662Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 371662
[Cl:1][C:2]1[CH:3]=[C:4]2[N:10]([OH:11])[C:9]([C:12]([F:15])([F:14])[F:13])=[N:8][C:5]2=[N:6][CH:7]=1.[CH2:16]([NH2:23])[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1>C(OCC)(=O)C>[CH2:16]([NH2:23])[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.[Cl:1][C:2]1[CH:3]=[C:4]2[N:10]([OH:11])[C:9]([C:12]([F:13])([F:14])[F:15])=[N:8][C:5]2=[N:6][CH:7]=1

Komponenten

4

Edukt 2

HCID 7504BenzylamineHCID 30824181-Hydroxyfluromidine

Produkt 1

HCID 203554646-chloro-1-hydroxy-2-(trifluoromethyl)-1H-imidazo(4,5-b)pyridine benzylamine salt

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

6-Chloro-1-hydroxy-2-(trifluoromethyl)-1H-imidazo(4,5-b)pyridine (1.4 grams) was mixed with 15 milliliters of ethyl acetate. The mixture was heated to reflux, and 0.6 milliliter of benzylamine was added dropwise. The mixture was then refluxed for another 30 minutes, cooled, and filtered, yielding the desired 6-chloro-1-hydroxy-2-(trifluoromethyl)-1H-imidazo(4,5-b)pyridine benzylamine salt, m.p., 200°-02° C. NMR analysis in hexadeuterodimethyl sulfoxide showed a peak at 236 cps (2H); a peak at 437 cps (5H); two meta-coupled doublets at the 462 cps (1H), the other at 500 cps (1H); and a broad peak at 474 cps (3H).

Aufarbeitung

  1. temperatureThe mixture was heated
  2. temperatureto reflux
  3. temperatureThe mixture was then refluxed for another 30 minutes
  4. temperaturecooled
  5. filtrationfiltered

Quellen und Nachweise

ORD-Eintrag
ord-23b99b59eb9943f987fd1061c19e183f
Quelldatensatz
uspto-grants-1978_05
Patentnummer
US04087432

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