Reaktion #438510

Reaktionsgleichung

dimethylamine hydrochloride

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

dimethylamine

potassium cyanide

→

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

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwere added
2. 2
   ExtraktionThe resultant white suspension was extracted four times with 800 ml diethylether in each case
3. 3
   Einengenthe combined extracts were initially concentrated
4. 4
   Sonstigethe organic phase was separated
5. 5
   Trocknendried over sodium sulfate
6. 6
   Filtrationfiltered
7. 7
   Einengenconcentrated

Vorschrift

Starting with 200 g 1,4-dioxaspiro[4.5]decan-8-one, 168 l aqueous dimethylamine solution (40% by volume), 200 ml methanol, 200 g potassium cyanide and 303 g dimethylamine hydrochloride were added and the reaction mixture was stirred for 65 hours at ambient temperature. The resultant white suspension was extracted four times with 800 ml diethylether in each case, the combined extracts were initially concentrated and taken up with 500 ml dichloromethane, the organic phase was separated, dried over sodium sulfate, filtered, concentrated and substantially freed of solvent residues under vacuum. 265 g 8-dimethylamino-1,4-dioxaspiro[4.5]decane-8-carbonitrile were obtained as a white solid.

Quelle