2,2,6,6-四甲基-4-甲氧基哌啶氮氧自由基制备方法的改进

Preparation of 4-Methoxy-2,2,6,6-Teramethylpiperidinyl-1-Oxy

阐述了一种制备 4 -甲氧基 -2 ,2 ,6 ,6 -四甲基哌啶氮氧自由基的改进方法 :以四氢呋喃为溶剂 ,0℃时 ,在N2 的保护下和NaH的存在下 ,2 ,2 ,6 ,6 -四甲基 -4 -羟基哌啶氮氧自由基与MeI在室温反应 5h。分离混合物 ,得到粘稠状红色液体 ,加入正己烷 ,在 -2 0℃条件下储存 ,结晶出针状深红色的晶体。熔点 :4 2～ 4 3℃ ,产率 70

A new route for the preparation of 4-Methoxy-2, 2, 6,6 - teramethylpiperidinyl-1-oxy has been developed, a stirred solution of 4-hydroxy-2, 2, 6, 6-tetramethylpiperidinyl-1-oxy in THF was added NaH. After this suspension was stirred under nitrogen, methyl iodide was added to the solution at 0 ℃.The reaction mixture stood at room temperature for 5 h. After filtration , n-Hexane was added and the mixture was stored at -20 ℃, red needle crystals were obtained. mp: 42～43 ℃,yield: More than 70 %.