Reaktion #977791

Reaktionsgleichung

dimethylamine

dimethylamine hydrochloride

potassium cyanide

1,4-dioxaspiro[4.5]decan-8-one

→

8-dimethylamino-1,4-dioxaspiro[4.5]decane-8-carbonitrile

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   ExtraktionThe resulting white suspension was extracted four times with 800 ml ether each time
2. 2
   Einengenthe combined extracts concentrated to low volume
3. 3
   Sonstigethe phases separated
4. 4
   TrocknenThe organic phase was dried over sodium sulfate
5. 5
   Filtrationfiltered
6. 6
   Einengenconcentrated to low volume

Vorschrift

200 ml methanol, 1680 ml aqueous dimethylamine solution (40 m %), 303 g dimethylamine hydrochloride and 200 g potassium cyanide were added to 200 g 1,4-dioxaspiro[4.5]decan-8-one and stirred for approximately 65 hours. The resulting white suspension was extracted four times with 800 ml ether each time, the combined extracts concentrated to low volume, the residue taken up in approximately 500 ml dichloromethane and the phases separated. The organic phase was dried over sodium sulfate, filtered and concentrated to low volume. 265 g 8-dimethylamino-1,4-dioxaspiro[4.5]decane-8-carbonitrile were obtained as a white solid.

Quelle