Реакция #511797

Уравнение реакции

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

Растворители

methanol

water

Условия реакции

Обработка

1. 1
   Температураwhile cooling with ice
2. 2
   Экстракцияextracted with diethyl ether (4×100 ml)
3. 3
   СушкаThe organic phase was dried over sodium sulfate
4. 4
   Концентрированиеconcentrated i
5. 5
   Другоеand the product was obtained as a white solid

Методика

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.

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