Water → 2-Ethyl-6-[3-(trifluoromethyl)phenyl]imidazo[1,2-b]pyridazine

HRID 1589461

Reaktionsgleichung

Reaktionsgleichung von HRID 1589461
Cl[C:2]1[N:3]=[N:4][C:5]([C:8]2[CH:13]=[CH:12][CH:11]=[C:10]([C:14]([F:17])([F:16])[F:15])[CH:9]=2)=[CH:6][CH:7]=1.O>NC(CC)CO>[CH2:6]([C:5]1[N:4]=[C:2]2[CH:7]=[CH:6][C:5]([C:8]3[CH:13]=[CH:12][CH:11]=[C:10]([C:14]([F:17])([F:16])[F:15])[CH:9]=3)=[N:4][N:3]2[CH:8]=1)[CH3:7]

Komponenten

4

Edukt 2

HCID 962WaterHCID 124495523-Chloro-6-[3-(trifluoromethyl)phenyl]pyridazine

Produkt 1

HCID 202465672-Ethyl-6-[3-(trifluoromethyl)phenyl]imidazo[1,2-b]pyridazine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 221292-Amino-1-butanolLösungsmittel

Versuchsvorschrift

A 2.58 g sample of 3-chloro-6-[3-(trifluoromethyl)phenyl]pyridazine in 3.56 g of 2-amino-1-butanol was heated at 120° C. (internal temperature) for 18 hours, cooled and poured into cold water. The mixture was extracted with dichloromethane and the extracts washed with water, dried over anhydrous sodium sulfate and concentrated. The residue in ethyl acetate was chromatographed on silica gel with ethyl acetate to give 2.2 g of yellow oil. Crystallization from dichloromethane-hexane gave 2-{[6-[3-(trifluoromethyl)phenyl]-3-pyridazinyl]amino}-1-butanol as crystals, mp 84°-87° C.

Aufarbeitung

  1. temperaturecooled
  2. extractionThe mixture was extracted with dichloromethane
  3. washthe extracts washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated
  6. customThe residue in ethyl acetate was chromatographed on silica gel with ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-2d8f46115af044c68d9b8ec912423530
Quelldatensatz
uspto-grants-1986_02
Patentnummer
US04569934

Verknüpfte Notizen

Wird geladen…