Reaktion #1266209

Reaktionsgleichung

dimethylamine

dimethylamine hydrochloride

potassium cyanide

1,4-dioxa-spiro[4.5]decan-8-one

→

8-dimethylamino-1,4-dioxa-spiro[4.5]decane-8-carbonitrile

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe white suspension obtained
2. 2
   Extraktionwas extracted four times with 800 ml ether each time
3. 3
   Einengenthe combined extracts were concentrated
4. 4
   Sonstigethe phases were separated
5. 5
   TrocknenThe methylene chloride phase was dried over sodium sulfate
6. 6
   Filtrationfiltered
7. 7
   Einengenconcentrated

Vorschrift

200 ml methanol, 1,680 ml aqueous dimethylamine solution (40 wt. %), 303 g dimethylamine hydrochloride and 200 g potassium cyanide were added to 200 g 1,4-dioxa-spiro[4.5]decan-8-one and the mixture was stirred for approx. 65 hours. The white suspension obtained was extracted four times with 800 ml ether each time, the combined extracts were concentrated, the residue was taken up in approx. 500 ml methylene chloride and the phases were separated. The methylene chloride phase was dried over sodium sulfate, filtered and concentrated. 265 g 8-dimethylamino-1,4-dioxa-spiro[4.5]decane-8-carbonitrile were obtained as a white solid.

Quelle