Perchloric Acid → Ethyl 3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate

HRID 345825Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 345825
O1CCCCC1[N:7]1[O:14][CH2:13][CH:12]2[CH:8]1[CH2:9][N:10]([C:15]([O:17][CH2:18][CH3:19])=[O:16])[CH2:11]2.Cl(O)(=O)(=O)=O.C[O-].[Na+]>C(O)C>[CH:8]12[CH2:9][N:10]([C:15]([O:17][CH2:18][CH3:19])=[O:16])[CH2:11][CH:12]1[CH2:13][O:14][NH:7]2

Komponenten

5

Edukt 3

HCID 24247Perchloric AcidHCID 10942334Sodium MethoxideHCID 15070014Ethyl 2-(tetrahydropyran-2-yl)-3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate

Produkt 1

HCID 15070015Ethyl 3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

15 g (55.5 mmol) of ethyl 2-(tetrahydropyran-2-yl)-3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate are heated under reflux with 8.25 g (56 mmol) of 70% strength perchloric acid in 100 ml of ethanol for 30 minutes. 10.5 g (58 mmol) of 30 strength sodium methylate solution are added, the mixture is concentrated, the residue is taken up in water and the solution is saturated with K2CO3 and extracted with CHCl3. The extract is dried over K2CO3 and concentrated and the residue is distilled.

Aufarbeitung

  1. concentrationthe mixture is concentrated
  2. extractionextracted with CHCl3
  3. dry with materialThe extract is dried over K2CO3
  4. concentrationconcentrated
  5. distillationthe residue is distilled

Quellen und Nachweise

ORD-Eintrag
ord-b086630863c84c9f886a925424f6dc3a
Quelldatensatz
uspto-grants-1991_10
Patentnummer
US05059597

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