反応 #511797

反応方程式

dimethylamine

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
   温度while cooling with ice
2. 2
   抽出extracted with diethyl ether (4×100 ml)
3. 3
   乾燥The organic phase was dried over sodium sulfate
4. 4
   濃縮concentrated i
5. 5
   その他and the product was obtained as a white solid

実験手順

40 percent strength aqueous dimethylamine solution (85 ml, 0.67 mol), 1,4-dioxa-spiro[4.5]decane-8-carbaldehyde (240 g, 0.141 mol) and potassium cyanide (22.05 g, 0.338 mol) were added to a mixture of 4 N hydrochloric acid (37 ml) and methanol (22 ml), while cooling with ice. The mixture was stirred at room temperature for 4 d and then, after addition of water (80 ml), extracted with diethyl ether (4×100 ml). The organic phase was dried over sodium sulfate and concentrated i. vac. and the product was obtained as a white solid. Yield: 25.2 g (81%), melting point: 48-51° C.

出典