反应详情

A solution of 2-[(3R)-3-fluoro-pyrrolidin-1-yl]-6-methyl-4-morpholin-4-yl-benzonitrile (0.18 g, 0.62 mmol) in sulphuric acid (8 ml) is heated at 100° C. for 1 h. After completion of the reaction (monitored by TLC), the mixture is poured onto ice water. The aqueous layer is basified with aqueous ammonia to pH 10 and extracted with ethyl acetate (3×20 ml). The combined organic layers are washed with water (10 ml), dried over sodium sulfate and concentrated in vacuo yielding 2-[(3R)-3-fluoro-pyrrolidin-1-yl]-6-methyl-4-morpholin-4-yl-benzamide (0.13 g, 0.423 mmol, 68%).

1. customAfter completion of the reaction (monitored by TLC)
2. additionthe mixture is poured onto ice water
3. extractionextracted with ethyl acetate (3×20 ml)
4. washThe combined organic layers are washed with water (10 ml)
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated in vacuo