Reaktion #4307
ord-b9ffe40dfc354894b3753bf7aa940b3d
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1SonstigeThe solvent was removed in vacuo
- 2Sonstigethe residue was partitioned between methylene chloride and dilute sodium hydroxide
- 3TrocknenThe methylene chloride phase was dried over magnesium sulfate
- 4Sonstigethe solvent was removed in vacuo
- 5Sonstigeto give an oil
- 6SonstigeA precipitate was collected
Vorschrift
A mixture of 51.4 g (0.253 mole) of 2-chloroethyl phenyl sulfone, 50.2 g (0.417 mole) of 3-ethoxy-1-propanamine, and 33.0 g (0.327 mole) of triethylamine in 400 ml of acetonitrile was stirred at room temperature for 20 hr. The solvent was removed in vacuo and the residue was partitioned between methylene chloride and dilute sodium hydroxide. The methylene chloride phase was dried over magnesium sulfate, and the solvent was removed in vacuo to give an oil. This was dissolved in methanol, an excess of ethereal hydrogen chloride was added and ether was added. A precipitate was collected to give 49.2 g (63.2%) of white crystalline solid, m.p. 169°-170° C.