反应详情

To a solution of 2-(4-oxo-piperidin-1-yl)-benzonitrile (5) (653 mg, 3.26 mmol) and 4 (890 mg, 3.58 mmol) in 40 ml of methanol was added 4 g of powdered 4 Å molecular sieves. The resulting suspension was stirred at room temperature for 24 hours. The suspension was subsequently acidified to pH 5 with acetic acid and a 1M solution of NaCNBH3 in THF (6.0 ml 5.6 mmol) was added slowly with a syringe pump over 24 hours. When the addition was complete, the solvent was removed in vacuo and the residue taken up in chloroform and filtered. The solution was then washed with 10% Na2CO3, dried over MgSO4, and the solvent removed in vacuo to give the crude amine. The crude product was purified by chromatography on silica gel (5% MeOH/CHCl3) to give the title compound.

1. additionWhen the addition
2. customthe solvent was removed in vacuo
3. filtrationfiltered
4. washThe solution was then washed with 10% Na2CO3
5. dry with materialdried over MgSO4
6. customthe solvent removed in vacuo
7. customto give the crude amine
8. customThe crude product was purified by chromatography on silica gel (5% MeOH/CHCl3)