Reaktion #836620

Reaktionsgleichung

8-[1-(Diphenylmethyl)azetidin-3-yl]-1,4-dioxa-8-azaspiro[4.5]decane

1-chloroethyl chloroformate

methanol

→

8-azetidin-3-yl-1,4-dioxa-8-azaspiro[4.5]decane hydrochloride

Ausbeute 73.0%

Lösungsmittel

—

resultant solution

CH2Cl2

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe solution was heated
2. 2
   Temperaturto reflux for 20 min
3. 3
   Sonstigethe solvent was removed by evaporation
4. 4
   SonstigeThe residue was triturated with acetone
5. 5
   Sonstigethe precipitate was then recrystallised from isopropyl alcohol

Vorschrift

8-[1-(Diphenylmethyl)azetidin-3-yl]-1,4-dioxa-8-azaspiro[4.5]decane (0.5 g, 1.4 mmol) was dissolved in dry CH2Cl2 under nitrogen and to the resultant solution was added 1-chloroethyl chloroformate (0.45 mL, 4.1 mmol) at 0° C. The mixture was stirred for 1.5 h and then methanol was added. The solution was heated to reflux for 20 min and then the solvent was removed by evaporation. The residue was triturated with acetone and the precipitate was then recrystallised from isopropyl alcohol. There was obtained 235 mg (73%) of 8-azetidin-3-yl-1,4-dioxa-8-azaspiro[4.5]decane hydrochloride as a solid. LCMS: m/z 199 (M+1)+.

Quelle