反应详情

To a suspension of 2.8 g of nicotinic acid 1-oxide, 2.5 g of dimethylaminopyridine, 8.8 g of benzotriazolyloxy-tris-(dimethylamino)phosphonium hexafluorophosphate in 40 ml of acetonitrile, 5 g of 3-[3-(3-methylpiperidinomethyl)phenoxy]propylamine dissolved in 10 ml of acetonitrile are added at 20° C. under stirring. A rising of the temperature up to 30° C. is observed and a solution is obtained which is then stirred 2 hours at room temperature. The mixture is concentrated under reduced pressure, the residue is treated with 20 ml of concentrated sodium hydroxide and extracted 4 times with 40 ml of ethyl acetate. After evaporation of the organic extracts, the residue is purified by chromatography on silica as described in Example 7. Thus, the N-[3-[3-(3-methylpiperidinomethyl)phenoxy]propyl]-3-pyridinecarboxamide 1-oxide is obtained, identical to the product of Example 8.

1. additionare added at 20° C.
2. customA rising of the temperature up to 30° C.
3. customa solution is obtained which
4. stirringis then stirred 2 hours at room temperature
5. concentrationThe mixture is concentrated under reduced pressure
6. additionthe residue is treated with 20 ml of concentrated sodium hydroxide
7. extractionextracted 4 times with 40 ml of ethyl acetate
8. customAfter evaporation of the organic extracts
9. customthe residue is purified by chromatography on silica