反应详情

6.5 g (180 mmol) N-[4-(piperidin-4-yl)-butyl]-3-(pyridin-3-yl)-acrylamide dihydrochloride (substance 22) are suspended in 80 ml acetone added to 9.9 g (72.0 mmol) potassium carbonate. A solution of 3.4 g (19.8 mmol) benzyl bromide in 10 ml acetone is added dropwise to this mixture at RT and stirred overnight. Subsequently, the suspension is filtered and the filtrate is concentrated under vacuum. The residue is taken up in 100 ml CHCl3 and washed with 30 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 to 90/10) and crystallized from 15 ml acetonitrile after drawing off the solvent. Beige colored crystals with a MP of 88-90° C. were recovered; yield: 1.1 g (16%).

1. filtrationSubsequently, the suspension is filtered
2. concentrationthe filtrate is concentrated under vacuum
3. washwashed with 30 ml water
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 to 90/10)
7. customcrystallized from 15 ml acetonitrile
8. customBeige colored crystals with a MP of 88-90° C. were recovered