反応 #644694

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 in vacuo
4. 4
   その他the product was obtained in the form of a white solid

実験手順

40% aqueous dimethylamine solution (85 ml, 0.67 mol), 1,4-dioxa-spiro[4.5]decane-8-carbaldehyde 2 (240 g, 0.141 mol) and potassium cyanide (22.05 g, 0.338 mol) were added, while cooling with ice, to a mixture of 4N hydrochloric acid (37 ml) and methanol (22 ml). The mixture was stirred for 4 d at room temperature 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 in vacuo, and the product was obtained in the form of a white solid.

出典