反应详情

温度

135 °C

A mixture of 4-(cyclohexylmethoxy)phenylacetonitrile (15 g, prepared in the preceding paragraph), sodium azide (21.3 g), ammonium chloride (17.4 g) and dimethylformamide (325 mL) was heated to 135° C. under a nitrogen atmosphere for 40 hours. The mixture was then cooled to room temperature and enough water was added to dissolve all the salts. The homogeneous solution was then poured into a separatory funnel containing saturated aqueous NaCl and ethyl acetate. After extraction of the aqueous phase with additional ethyl acetate, the combined extracts were washed with saturated brine solution, dried over MgSO4 and concentrated. The dark amber oil so obtained was treated with a little water and the resulting solid filtered off and crystallized from dichloromethane-diethyl ether mixture to afford 10.5 g (59% yield) of the title compound; m.p. 156°-158° C.

1. temperatureThe mixture was then cooled to room temperature
2. dissolutionto dissolve all the salts
3. additionThe homogeneous solution was then poured into a separatory funnel
4. extractionAfter extraction of the aqueous phase with additional ethyl acetate
5. washthe combined extracts were washed with saturated brine solution
6. dry with materialdried over MgSO4
7. concentrationconcentrated
8. customThe dark amber oil so obtained
9. filtrationthe resulting solid filtered off
10. customcrystallized from dichloromethane-diethyl ether mixture