Benzyl Bromide → Ethyl alpha-benzylacetoacetate

HRID 898497

Reaktionsgleichung

Reaktionsgleichung von HRID 898497
[C:1]([O:7][CH2:8][CH3:9])(=[O:6])[CH2:2][C:3]([CH3:5])=[O:4].C([O-])([O-])=O.[K+].[K+].[CH2:16](Br)[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.[NH4+].[Cl-]>C1C=CC=CC=1>[CH2:16]([CH:2]([C:3](=[O:4])[CH3:5])[C:1]([O:7][CH2:8][CH3:9])=[O:6])[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1

Komponenten

6

Edukt 4

HCID 7498Benzyl BromideHCID 8868Ethyl AcetoacetateHCID 11430Potassium CarbonateHCID 25517Ammonium Chloride

Produkt 1

HCID 246929Ethyl alpha-benzylacetoacetateAusbeute 74 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 241BenzeneLösungsmittel

Versuchsvorschrift

0.1 Mol of ethyl acetoacetate, 0.1 mol of K2CO3, 0.1 mol of benzyl bromide, 0.01 mmol of PEG-400 (polyethylene glycol 400) and 100 ml of benzene were stirred at 75° C. for 7 hours. After cooling, 20 ml of saturated solution of NH4Cl was added to dissolve solid, and product was extracted with ethyl acetate. After removing the solvent, the residue was distilled under reduced pressure, and a cut fraction was collected at 116-118° C./20 Pa. Yield 74%.

Aufarbeitung

  1. temperatureAfter cooling
  2. dissolutionto dissolve solid, and product
  3. extractionwas extracted with ethyl acetate
  4. customAfter removing the solvent
  5. distillationthe residue was distilled under reduced pressure
  6. customa cut fraction was collected at 116-118° C./20 Pa

Quellen und Nachweise

ORD-Eintrag
ord-e2405c4aecdd42af8025950385979ec4
Quelldatensatz
uspto-grants-2008_04
Patentnummer
US07351778B2

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