反应详情

温度

60 °C

A mixture of 4-amino-1-Boc-piperidine (commercial; 6.7 g, 35 mmol), 2-chloro-6-methoxy-3-nitro-pyridine (1 eq.) and K2CO3 (1 eq.) in MeCN (100 mL) and DMF (30 mL) was heated at 60° C. for 3 h. The mixture was filtered and concentrated in vacuo. The residue was taken up in ether/water 1:1, the org. phase dried over MgSO4 and concentrated. The residue was triturated with EA and filtered to afford 4.5 g of pure product. The filtrate was concentrated and purified by CC (Hept/EA 9:1, 4:1, 2:1) to give another 4 g of product. In total 8.5 g (70% yield) of a yellow solid were obtained.

1. filtrationThe mixture was filtered
2. concentrationconcentrated in vacuo
3. dry with materialphase dried over MgSO4
4. concentrationconcentrated
5. customThe residue was triturated with EA
6. filtrationfiltered