Reaktion #824285
ord-d496930bdc2143efb06afa27cc8a3d3c
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
60°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1SonstigeThe solvent could be removed in vacuo and 1N aqueous hydrogen chloride solution
- 2workup.ADDITIONcould be added to the resulting residue
- 3Waschenthe mixture could be washed with diethyl ether
- 4workup.ADDITIONThe aqueous layer could be adjusted to pH 14 by addition of 2N NaOH solution
- 5Extraktionextracted with methylene chloride
- 6WaschenThe organic layer could be washed with brine
- 7Trocknendried over sodium sulfate
- 8FiltrationAfter filtering
- 9Sonstigethe material could be purified by column chromatography
Vorschrift
The above compound could be made in the following manner: 1 eq. 2-Benzyl-morpholine-4-carboxylic acid tert-butyl ester could be dissolved in 4N solution of hydrogen chloride in dioxane and the mixture could be stirred at 60° C. for 3 h. The solvent could be removed in vacuo and 1N aqueous hydrogen chloride solution could be added to the resulting residue, and the mixture could be washed with diethyl ether. The aqueous layer could be adjusted to pH 14 by addition of 2N NaOH solution and extracted with methylene chloride. The organic layer could be washed with brine and dried over sodium sulfate. After filtering, the material could be purified by column chromatography.