反应详情

温度

100 °C

5-Chloro-3-cyclopentyloxy-2-nitro-pyridine (0.8 mmol) is dissolved in DMF (8 ml), phenol (3 eq.) and K2CO3 (4 eq.) is added. The reaction mixture is heated to 100° C. in the microwave for 60 min. The reaction solution is pored into water and extracted with methyl-tert.-butyl ether. The combined organic layers are washed with brine, dried over MgSO4 and the solvent is removed in vacuo. 3-Cyclopentyloxy-2-nitro-5-phenoxy-pyridine is obtained after column chromatography (heptane/ethyl acetate) as yellow oil in a yield of 60%; HPLC (method C): 2.23 min; LC-MS (method A): 2.31 min, 301.15 (M+H+).

1. extractionextracted with methyl-tert.-butyl ether
2. washThe combined organic layers are washed with brine
3. dry with materialdried over MgSO4
4. customthe solvent is removed in vacuo