HRID69875
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
A heterogeneous solution of 4-cyclohexenyl-3-nitropyridine (1.0 eq.) and iron (6.0 eq) in acetic acid, at a concentration of 0.4 M, was stirred vigorously for 2 hours. The mixture was then passed through a celite pad, eluting with MeOH. Upon removal of the volatiles in vacuo, the residue was dissolved in EtOAc, washed with Na2CO3(sat.), NaCl(sat.), was dried over MgSO4, was filtered and the volatiles were removed in vacuo yielding 4-cyclohexenylpyridin-3-amine (99%) as an oil. LCMS (m/z): 175.0 (MH+); LC Rt=1.86 min.
WORKUP
后处理
- washeluting with MeOH
- customUpon removal of the volatiles in vacuo
- dissolutionthe residue was dissolved in EtOAc
- washwashed with Na2CO3(sat.), NaCl(sat.)
- dry with materialwas dried over MgSO4
- filtrationwas filtered
- customthe volatiles were removed in vacuo