反应详情

温度

180 °C

Sodium triacetoxyborohydride (100 mg, 3.9 mol eq) was added to a solution of 1-chloro-6-(piperidin-3-yloxy)isoquinoline (40mg), acetic acid (1 drops) and benzaldehyde (40 μl) in N, N-dimethylformamide (0.5 ml) and shaken for 17 hours. The reactions were quenched with water (0.5 ml) and shaken for 1 h then loaded onto a pre-acidified SCX column using methanol and eluted with 2M ammonia in methanol. The product was concentrated in vacuo to give a residue which was treated with 5M aqueous hydrochloric acid and heated in the microwave at 180° C. for 60 minutes. The mixture was concentrated in vacuo to give a residue which was purified by prep-HPLC to give 6-(1-benzylpiperidin-3-yloxy)-2H-isoquinolin-1-one, El-MS: m/z=335.7 [M+H]+.

1. customThe reactions were quenched with water (0.5 ml)
2. stirringshaken for 1 h
3. washeluted with 2M ammonia in methanol
4. concentrationThe product was concentrated in vacuo
5. customto give a residue which
6. concentrationThe mixture was concentrated in vacuo
7. customto give a residue which
8. customwas purified by prep-HPLC