Reaktion #54664
ord-d4a83106185d4c60b359d7037c4b05d9
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1TemperaturThe reaction mixture becomes warm
- 2Sonstigefinally a yellow oil starts to separate out
- 3workup.ADDITIONwas poured into water
- 4SonstigeThe organic layer was separated
- 5Waschenwashed with dilute H2SO4
- 6Trocknendried (MgSO4)
- 7SonstigeRemoval of the solvent
- 8workup.WAITleft a viscous oil (3.8 g.)
- 9workup.DISTILLATIONThis was distilled under vacuum
Vorschrift
A solution of p-menth-3-oyl chloride prepared as in Example 1 (4.0g., 0.020 moles) in chloroform (30 ml.) was added dropwise to a stirred solution of ethanolamine (3 g., 0.043 moles) in chloroform (50 ml.). The reaction mixture becomes warm, goes cloudy and finally a yellow oil starts to separate out. After stirring for 2 hours at room temperature the mixture was poured into water. The organic layer was separated, washed with dilute H2SO4, and dried (MgSO4). Removal of the solvent left a viscous oil (3.8 g.). This was distilled under vacuum to yield N-(2-hydroxyethyl)-p-menthane-3-carboxamide as a colourless very viscous oil, b.p. 160°/01. mm.