1-丙氧基-2,2,6,6-四甲基哌啶醇的合成

Synthesis of 1-propoxy-2,2,6,6-tetramethylpiperidine-4-ol

以4-羟基-2,2,6,6-四甲基哌啶氮氧自由基(ZJ-701)和正丁醛为原料,质量分数30%的H_2O_2为氧化剂,CuCl为还原剂,通过O-烷基化反应合成了1-丙氧基-2,2,6,6-四甲基哌啶醇,并通过红外光谱、核磁共振氢谱、核磁共振碳谱和质谱表征了其结构。结果表明,其较佳工艺条件为n(ZJ-701)∶n(正丁醛)∶n(H_2O_2)∶n(CuCl)=1∶3.56∶2.80∶0.045,烷基化反应温度20℃,烷基化反应时间12h。在上述条件下合成的产品通过重结晶,产品的质量分数可达96.6%,熔点为61～62℃,分离产率超过69%。

1-Propoxy-2,2,6,6-tetramethylpiperidine-4-ol was synthesized through O-alkylation by using4-hydroxy-2,2,6,6-tetramethyl-piperidinooxy(ZJ-701)and n-butyraldehyde as raw materials,30%H2O2as oxidant,CuCl as reducing agent,and its structure was characterized by IR,1H NMR,13C NMR and MS.The results revealed that its optimal conditions were as follows:n(ZJ-701)∶n(n-butylaldehyde)∶n(H2O2)∶n(CuCl)=1∶3.56∶2.80∶0.045,the alkylation time being 12h,and the alkylation temperature being 20℃.The weight fraction of the product was 96.6%,the melting point was61~62℃ and the separation yield was over 69% by recrystallization of the crude products obtained under the optimal conditions.