1-环己氧基-4-羟基-2,2,6,6-四甲基哌啶醇的合成

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

对以4-羟基-2,2,6,6-四甲基哌啶氮氧自由基(ZJ-701)和环己烷为原料,叔丁基过氧化氢为氧化剂,CuCl_2·2H_2O为催化剂,通过O-烷基化反应合成1-环己氧基-4-羟基-2,2,6,6-四甲基哌啶醇进行了研究。结果表明,较佳反应条件为:n(ZJ-701)∶n(TBHP)∶n(CuCl_2)∶n(环己烷)∶n(乙醇)=1∶9.6∶0.25∶13∶35,反应时间为9h,反应温度约65℃,较理想的提纯工艺为硼氢化物还原-减压蒸馏-重结晶。在以上条件下,目标产物的含量为98.49%,分离产率为52.0%。该工艺反应条件温和,产品含量及收率较高。

1-Cyclohexyloxy-2,2,6,6-tetramethylpiperidine-4-ol was synthesized by O-alkylation reaction by using 4-hydroxy-2,2,6,6-tetramethyl-piperidinooxy（（ZJ-701）and cyclohexane as raw materials,tert-butyl hydroperoxide（TBHP）as oxidant,CuCl2 as catalyst.The results revealed that its optimal conditions were as follows：n（ZJ-701）∶n（TBHP）∶n（CuCl2）∶n（cyclohexane）∶n（ethanol）= 1∶9.6∶0.25∶13∶35,the reaction time being9 h,and the reaction temperature being 65 ℃,and optimal separation process was borohydride reduction-vacuum distillation-recrystallation.Under the above conditions,the separated yield of the products was 52.0% and the purity was 98.49%.The process has some advantages such as mild reaction condition,higher yield and purity.