反应详情

3.48 ml (30 mmol) benzoyl chloride, 8.7 g (30 mmol) N-(4-piperidin-4-yl-butyl)-3-(pyridin-3-yl)-propionamide and 16.6 g (120 mmol) potassium carbonate are stirred in 160 ml DMF at RT overnight. Subsequently, this is filtered and the filtrate is concentrated under vacuum to a large extent. The residue is taken up in 400 ml CHCl3 and washed twice, each with 100 ml water. The organic phase is dried over sodium sulfate and the solvent is removed under vacuum. The residue is chromatographically purified over silica gel with CHCl3/CH3OH (95/5) and precipitates as an amorphous solid after drawing off the solvent.

1. filtrationSubsequently, this is filtered
2. concentrationthe filtrate is concentrated under vacuum to a large extent
3. washwashed twice
4. dry with materialThe organic phase is dried over sodium sulfate
5. customthe solvent is removed under vacuum
6. customThe residue is chromatographically purified over silica gel with CHCl3/CH3OH (95/5)
7. customprecipitates as an amorphous solid