HRID69870
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
PROCEDURE
实验过程
3-bromo-4-nitropyridine-N-oxide (1.0 equiv.) and piperidine (2.0 equiv.) in ethanol, at a concentration of 0.2 M, was heated at reflux for 16 hours. Upon cooling the ethanol was removed in vacuo. The residue was partitioned between EtOAc and Na2CO3(sat), and washed further with H2O, NaCl(sat.), was dried over MgSO4, was filtered and the volatiles were removed in vacuo yielding 4-nitro-3-(piperidin-1-yl)pyridine 1-oxide (92%). LCMS (m/z): 224.0 (MH+); LC Rt=2.48 min.
WORKUP
后处理
- temperatureat reflux for 16 hours
- customwas removed in vacuo
- customThe residue was partitioned between EtOAc and Na2CO3(sat)
- washwashed further with H2O, NaCl(sat.)
- dry with materialwas dried over MgSO4
- filtrationwas filtered
- customthe volatiles were removed in vacuo