반응 #438510

반응 방정식

dimethylamine hydrochloride

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

dimethylamine

potassium cyanide

→

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

용매

methanol

반응 조건

후처리

1. 1
   workup.ADDITIONwere added
2. 2
   추출The resultant white suspension was extracted four times with 800 ml diethylether in each case
3. 3
   농축the combined extracts were initially concentrated
4. 4
   기타the organic phase was separated
5. 5
   건조dried over sodium sulfate
6. 6
   여과filtered
7. 7
   농축concentrated

실험 절차

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.

출처