反应详情

温度

80 °C

To a stirred solution of 2-(ethylsulfinyl)-6-methyl-4-morpholin-4-yl-benzonitrile (0.78 g, 2.81 mmol) in ethanol (8.5 ml) is added a 5M solution of sodium hydroxide (8.5 ml) and the mixture is heated at 80° C. for 16 h. After completion of the reaction (monitored by TLC) the reaction mixture is concentrated to get a residue, which is diluted with water (10 ml) and extracted with ethyl acetate (3×30 ml). The combined organic layers are washed with water (10 ml), brine (10 ml), dried over anhydrous sodium sulfate and evaporated to get the crude product which is purified by column chromatography (alumina, 5% methanol/dichloromethane) to yield 2-(ethylsulfinyl)-6-methyl-4-morpholin-4-yl-benzamide (0.30 g, 1.01 mmol, 36%).

1. customAfter completion of the reaction (monitored by TLC) the reaction mixture
2. concentrationis concentrated
3. customto get a residue, which
4. extractionextracted with ethyl acetate (3×30 ml)
5. washThe combined organic layers are washed with water (10 ml), brine (10 ml)
6. dry with materialdried over anhydrous sodium sulfate
7. customevaporated
8. customto get the crude product which
9. customis purified by column chromatography (alumina, 5% methanol/dichloromethane)