Butanal → n-Butanal dicrotyl acetal

HRID 482144

Reaktionsgleichung

Reaktionsgleichung von HRID 482144
[CH:1](=[O:5])[CH2:2][CH2:3][CH3:4].[CH2:6]([OH:10])[CH:7]=[CH:8][CH3:9]>C/C(/O)=C/C(C)=O.C/C(/O)=C/C(C)=O.C/C(/O)=C/C(C)=O.C/C(/O)=C/C(C)=O.[Ti].C1(C)C=CC=CC=1>[CH2:1]([O:5][CH:6]([O:10][CH2:1][CH:2]=[CH:3][CH3:4])[CH2:7][CH2:8][CH3:9])[CH:2]=[CH:3][CH3:4]

Komponenten

5

Edukt 2

HCID 261ButanalHCID 200242-Buten-1-ol

Produkt 1

HCID 57271298n-Butanal dicrotyl acetalAusbeute 190,7 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 44629996tetrakis((Z)-4-hydroxypent-3-en-2-one);titaniumKatalysatorHCID 1140TolueneLösungsmittel

Reaktionsbedingungen

Temperatur
20 °C

Versuchsvorschrift

In a 300-ml three-necked flask, 72 g (1 mole) of n-butanal, 144 g of crotyl alcohol, 3 mg of titanium acetylacetonate, 80 g of molecular sieve 4A and 50 g of toluene were charged. The resulting mixture was stirred at 20° C. under atmospheric pressure for 12 hours in a nitrogen atmosphere. After the removal of the molecular sieve 4A from the reaction mixture, the solvent (toluene) and the unreacted starting materials were distilled off under reduced pressure. Distillation of the residue under reduced pressure gave 189.1 g of n-butanal dicrotyl acetal (boiling point: 116° C./25 mmHg) (yield: 95.5%).

Aufarbeitung

  1. customAfter the removal of the molecular sieve 4A from the reaction mixture
  2. distillationthe solvent (toluene) and the unreacted starting materials were distilled off under reduced pressure
  3. distillationDistillation of the residue under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-1083e6383f0346da8a1eb6f0d2893a8a
Quelldatensatz
uspto-grants-1998_08
Patentnummer
US05792876

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