Reaktion #1804392

Reaktionsgleichung

1,1-dimethylethyl (2R,5R)-2-(4-{[(2-fluorophenyl)methyl]oxy}phenyl)-6-oxo-1,7-diazaspiro[4.4]nonane-1-carboxylate

acetyl chloride

→

title compound

Ausbeute 92.0%

(2R,5R)-2-(4-{[(2-Fluorophenyl)methyl]oxy}phenyl)-1,7-diazaspiro[4.4]nonan-6-one hydrochloride

Ausbeute 92.0%

Lösungsmittel

AcOEt

MeOH

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.WAITat ambient temperature for 16 hours
2. 2
   SonstigeSolvent was evaporated (bath temperature
3. 3
   Sonstigefirst ambient and then 38° C.) and the residue solid was triturated with Et2O (3×244 mL)
4. 4
   FiltrationFinally the solid was collected by filtration
5. 5
   Sonstigedried under high vacuum at 35° C. overnight

Vorschrift

To a solution of 1,1-dimethylethyl (2R,5R)-2-(4-{[(2-fluorophenyl)methyl]oxy}phenyl)-6-oxo-1,7-diazaspiro[4.4]nonane-1-carboxylate (D26, 29.3 g) in AcOEt (325 mL) and MeOH (108 mL) at 0° C., was added acetyl chloride (28.5 mL). The resulting solution was stirred at 0° C. for 15 minutes then at ambient temperature for 16 hours. Solvent was evaporated (bath temperature: first ambient and then 38° C.) and the residue solid was triturated with Et2O (3×244 mL). Finally the solid was collected by filtration and dried under high vacuum at 35° C. overnight to afford the title compound (23 g, Y=92%) as white solid.

Quelle