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Ethyl 3-bromopropionate → HCID 20491693, Verbindung

HRID 1154030
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1154030
[Na].[O:2]=[C:3]1[N:7]2[CH2:8][CH2:9][CH2:10][CH:11]([C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[N:6]2[C:5](=[O:19])[CH2:4]1.Br[CH2:21][CH2:22][C:23]([O:25][CH2:26][CH3:27])=[O:24]>C(O)C>[CH2:26]([O:25][C:23]([CH2:22][CH2:21][C:4]1([CH2:10][CH2:11][C:12]([O:14][CH2:15][CH3:16])=[O:13])[C:3](=[O:2])[N:7]2[CH2:8][CH2:9][CH2:10][CH:11]([C:12]([O:14][C:15]([CH3:16])([CH3:18])[CH3:17])=[O:13])[N:6]2[C:5]1=[O:19])=[O:24])[CH3:27]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 68320Ethyl 3-bromopropionateHCID 5360545SodiumHCID 13774859HCID 13774859, Verbindung

Produkt 1

HCID 20491693HCID 20491693, VerbindungAusbeute 18,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel2×

Versuchsvorschrift

(b) 0.43 g of sodium was dissolved in 20 ml of ethanol. A solution of 2.27 g of tert.butyl hexahydro-1,3-dioxo-1H-pyrazolo[1,2-a]pyridazine-5-carboxylate in 20 ml of ethanol was added and the mixture was heated under reflux for 2 hours. 5 g of ethyl 3-bromopropionate were added and the mixture was heated under reflux for an additional 2 hours. The solvent was removed and the residue was partitioned between dichloromethane and 2N hydrochloric acid. The organic layer was separated and evaporated. The residue was chromatographed on silica gel to give 0.37 g (9%) of tert.butyl 2,2-bis(2-ethoxycarbonylethyl)-hexahydro-1,3-dioxo-1H-pyrazolo[1,2-a]pyridazine-5-carboxylate in the form of an oil.

Aufarbeitung

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 2 hours
  3. temperaturethe mixture was heated
  4. temperatureunder reflux for an additional 2 hours
  5. customThe solvent was removed
  6. customthe residue was partitioned between dichloromethane and 2N hydrochloric acid
  7. customThe organic layer was separated
  8. customevaporated
  9. customThe residue was chromatographed on silica gel

Quellen und Nachweise

ORD-Eintrag
ord-669e88fc5ffc4fa696f320aeb0e62563
Quelldatensatz
uspto-grants-1984_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04487929

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