HRID1966242
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
5-Chloro-3-cyclopentylmethoxy-2-nitro-pyridine (1.3 mmol) is dissolved in DMF (10 ml), phenol (3 eq.) and K2CO3 (4 eq.) is added. The reaction is heated to 100° C. in the microwave for 45 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-Cyclopentylmethoxy-2-nitro-5-phenoxy-pyridine is obtained after column chromatography (heptane/ethyl acetate) as yellow oil in a yield of 94%. HPLC (method C): 2.31 min; LC-MS (method A): 2.48 min, 315.15 (MH+).
WORKUP
后处理
- extractionextracted with methyl-tert.-butyl ether
- washThe combined organic layers are washed with brine
- dry with materialdried over MgSO4
- customthe solvent is removed in vacuo