反应详情

温度

70 °C

To a solution of acetonitrile (1.35 ml) in tetrahydrofuran (80 ml), cooled to 5° C., was added sodium hydride (0.94 g, 60% dispersion in oil). The mixture was stirred for 30 minutes before the addition of a solution of methyl 4-(morpholin-4-ylmethyl)benzoate (5.53 g) in tetrahydrofuran (20 ml). The resulting mixture was heated to 70° C. for 5 h. The mixture was cooled, quenched with saturated ammonium chloride (20 ml) and extracted with ethyl acetate. The organic extracts were dried (MgSO4) and evaporated to give a gum which was purified by column chromatography eluting with a 20–100% ethyl acetate/iso-hexane gradient to give 3-[4-(morpholin-4-ylmethyl)phenyl]-3-oxopropanenitrile (0.97 g).

1. temperatureThe mixture was cooled
2. customquenched with saturated ammonium chloride (20 ml)
3. extractionextracted with ethyl acetate
4. dry with materialThe organic extracts were dried (MgSO4)
5. customevaporated
6. customto give a gum which
7. customwas purified by column chromatography
8. washeluting with a 20–100% ethyl acetate/iso-hexane gradient