Pyridine → HCID 20028798, Verbindung

HRID 1722414

Reaktionsgleichung

Reaktionsgleichung von HRID 1722414
[CH2:1]([CH:4]1[CH2:9][C:8](=[O:10])[O:7][C:5]1=O)[CH:2]=[CH2:3].[Na].[N:12]1C=C[CH:15]=[CH:14][CH:13]=1>C(OCC)C>[CH2:13]([N:12]1[C:8](=[O:10])[CH2:9][CH:4]([CH2:1][CH:2]=[CH2:3])[C:5]1=[O:7])[CH:14]=[CH2:15]

Komponenten

5

Edukt 3

HCID 1049PyridineHCID 1110093-Allyl(dihydro)furan-2,5-dioneHCID 5360545Sodium

Produkt 1

HCID 20028798HCID 20028798, VerbindungAusbeute 89,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

About 140 g (1 mol) of allylsuccinic anhydride and 250 ml of diethyl ether which has been dried over metallic sodium are placed under nitrogen in a round-bottomed flask equipped with a stirrer, dropping funnel and reflux condenser, and then mixed with 75 g (0.95 mol) of pyridine. About 57 g of allylamine in 100 ml of diethyl ether which has been dried over metallic sodium are then added dropwise to the flask with stirring over a period of 2 hours. When the addition is complete, the mixture is refluxed for an additional 1 hour. The resultant mixture is washed in a separating funnel with 5 percent aqueous hydrochloric acid until the pH of the aqueous phase is 6.5. The organic phase is dried over magnesium sulfate. After filtering off the drying agent, the solvent is removed at 15 hPa (abs.). About 153 g of N-allyl-allylsuccinimide, which boils at 130° C. at 0.5 hPa, are obtained from the residue by distillation.

Aufarbeitung

  1. customare placed under nitrogen in a round-bottomed flask
  2. customequipped with a stirrer
  3. temperaturereflux condenser
  4. dry with materialAbout 57 g of allylamine in 100 ml of diethyl ether which has been dried over metallic sodium
  5. additionare then added dropwise to the flask
  6. additionWhen the addition
  7. temperaturethe mixture is refluxed for an additional 1 hour
  8. washThe resultant mixture is washed in a separating funnel with 5 percent aqueous hydrochloric acid until the pH of the aqueous phase
  9. dry with materialThe organic phase is dried over magnesium sulfate
  10. filtrationAfter filtering off the drying agent
  11. customthe solvent is removed at 15 hPa (abs.)

Quellen und Nachweise

ORD-Eintrag
ord-c1f7fbf6679b43378244b70c39153c3a
Quelldatensatz
uspto-grants-1989_08
Patentnummer
US04855378

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