반응 #40915

반응 방정식

dimethylamine

1,4-dioxa-spiro-[4.5]decane-8-carbaldehyde

1,4-dioxa-spiro[4.5]decane-8-carbaldehyde

potassium cyanide

hydrochloric acid

→

dimethylamino-(1,4-dioxa-spiro[4.5]dec-8-yl)-acetonitrile

용매

methanol

반응 조건

후처리

1. 1
   추출extracted
2. 2
   workup.ADDITIONafter adding water (80 ml)
3. 3
   건조The organic phase was dried over sodium sulfate
4. 4
   농축concentrated by evaporation in vacuo
5. 5
   기타the product was obtained as a white solid

실험 절차

40% aqueous dimethylamine solution (85 ml, 0.67 mole), 1,4-dioxa-spiro-[4.5]decane-8-carbaldehyde 5 (240 g, 0.141 mole) and potassium cyanide (22.05 g, 0.338 mole) were added while cooling with ice to a mixture of 4N hydrochloric acid (37 ml) and methanol (22 ml). The mixture was stirred for four days at room temperature and then extracted, after adding water (80 ml), with diethyl ether (4×100 ml). The organic phase was dried over sodium sulfate, concentrated by evaporation in vacuo, and the product was obtained as a white solid.

출처