反応 #40919

反応方程式

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

溶媒

methanol

water

反応条件

後処理

1. 1
   抽出extracted with diethyl ether (4×100 ml)
2. 2
   乾燥The organic phase was dried over sodium sulfate
3. 3
   濃縮concentrated by evaporation in vacuo
4. 4
   その他the product was obtained as a white solid

実験手順

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, after adding water (80 ml), extracted 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.

出典