Climbazole → 1-(4-Chlorophenoxy)-1-(1H-imidazol-1-yl)-3,3-dimethylbutan-2-ol

HRID 1758081

Reaktionsgleichung

Reaktionsgleichung von HRID 1758081
[Cl:1][C:2]1[CH:20]=[CH:19][C:5]([O:6][CH:7]([N:14]2[CH:18]=[CH:17][N:16]=[CH:15]2)[C:8](=[O:13])[C:9]([CH3:12])([CH3:11])[CH3:10])=[CH:4][CH:3]=1.C(O)=O.C(N(CC)CC)C>>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:6][CH:7]([N:14]2[CH:18]=[CH:17][N:16]=[CH:15]2)[CH:8]([OH:13])[C:9]([CH3:11])([CH3:12])[CH3:10])=[CH:19][CH:20]=1

Komponenten

3

Edukt 2

HCID 37907ClimbazoleHCID 11084032Triethylammonium formate

Produkt 1

HCID 1714401-(4-Chlorophenoxy)-1-(1H-imidazol-1-yl)-3,3-dimethylbutan-2-olAusbeute 56 %

Versuchsvorschrift

14 g (0.048 mol) of 1-(4-chlorophenoxy)-3,3-dimethyl-1-(imidazol-1-yl)-butan-2-one and 61.8 g (0.143 mol) of formic acid/triethylamine (5:2 addition compound) were heated at 145° C. for 4 hours. The reaction mixture was allowed to cool and was concentrated in vacuo. The residue was taken up in dilute sodium hydroxide solution and the mixture was extracted with methylene chloride. The organic phase was washed with water, dried over sodium sulphate and concentrated in vacuo. The residue was suspended in hot cyclohexane, the suspension was filtered hot and the solid was dried. 7.9 g (56% of theory) of 1-(4-chlorophenoxy)-3,3-dimethyl-1-(imidazol-1-yl)-butan-2-ol of melting point 145°-147° C. were obtained.

Aufarbeitung

  1. temperatureto cool
  2. concentrationwas concentrated in vacuo
  3. extractionthe mixture was extracted with methylene chloride
  4. washThe organic phase was washed with water
  5. dry with materialdried over sodium sulphate
  6. concentrationconcentrated in vacuo
  7. filtrationthe suspension was filtered hot
  8. customthe solid was dried

Quellen und Nachweise

ORD-Eintrag
ord-02f111901faa45cf844be6429bc0bf42
Quelldatensatz
uspto-grants-1983_02
Patentnummer
US04371700

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