Sodium Hydroxide → HCID 14349631, Verbindung

HRID 329940

Reaktionsgleichung

Reaktionsgleichung von HRID 329940
[OH-].[Na+].[OH:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[C:10]([N:12]1[CH:16]=[CH:15][N:14]=[CH:13]1)=[CH2:11].Cl[CH2:18][C:19]([CH3:23])=[C:20]([CH3:22])[CH3:21]>CO>[CH3:18][C:19](=[C:20]([CH3:22])[CH3:21])[CH2:23][O:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[C:10]([N:12]1[CH:16]=[CH:15][N:14]=[CH:13]1)=[CH2:11]

Komponenten

5

Edukt 3

HCID 14798Sodium HydroxideHCID 28055362-[1-(1H-imidazol-1-yl)vinyl]phenolHCID 122407322-Butene, 1-chloro-2,3-dimethyl-

Produkt 1

HCID 14349631HCID 14349631, VerbindungAusbeute 63 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

9.2 g (0.23 mol) of sodium hydroxide are added to a mixture of 39.1 g (0.21 mol) of 1-[1-(2-hydroxyphenyl)-vinyl]-imidazole and 200 ml of methanol at room temperature, with stirring. When the addition has ended, the mixture is stirred at 50° C. for a further 30 minutes and is then concentrated under reduced pressure by stripping off the solvent. The solid residue which remains is taken up in 200 ml of dimethylformamide. 24.9 g (0.21 mol) of 1-chloro-2,3-dimethyl-but-2-ene are added to the solution formed at a temperature of 25° C., with stirring. The reaction mixture is stirred at 20° C. for a further 12 hours and then worked up by being concentrated by stripping off the diluent. The residue obtained is chromatographed over silica gel. 35.5 g (63% of theory) of 1-[1-(2-(2,3-dimethyl-but-2-en-1-yl-oxy)phenyl)-vinyl]-imidazole in the form of an oil are obtained in this manner.

Aufarbeitung

  1. additionWhen the addition
  2. stirringthe mixture is stirred at 50° C. for a further 30 minutes
  3. concentrationis then concentrated under reduced pressure
  4. customformed at a temperature of 25° C.
  5. stirringwith stirring
  6. stirringThe reaction mixture is stirred at 20° C. for a further 12 hours
  7. concentrationby being concentrated
  8. customThe residue obtained
  9. customis chromatographed over silica gel

Quellen und Nachweise

ORD-Eintrag
ord-c0ab425eb82c45c8ab1134fb16dd1688
Quelldatensatz
uspto-grants-1990_01
Patentnummer
US04894381

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