3,4-O-亚异丙基吡哆醛的催化氧化合成工艺研究

Synthesis of 3,4-o-isopropylidene pyridoxal via catalytic oxidation

以分子氧为氧化剂、含Ni类水滑石为催化剂,研究了盐酸西氯他宁中间体3,4-O-亚异丙基吡哆醛的催化氧化合成工艺。结果表明,在原料3,4-O-亚异丙基吡哆醇物质的量为2 mmol、Ni2MgGa类水滑石催化剂质量为1.0 g、均三甲苯溶剂用量为8 mL、氧气流量为10 mL/min、反应温度为110℃、反应时间为6 h的条件下,3,4-O-亚异丙基吡哆醛的收率达到93.3%。

The catalytic oxidative process for the synthesis of 3,4-O-isopropylidene pyridoxal,which is the key intermediate for the production of cilotanin hydrochloride,is studied by using Ni-containing hydrotalcite as catalyst and using molecular oxygen as the oxidant.The results indicate that the yield of 3,4-O-isopropylidene pyridoxal reaches 93.3%under the optimized conditions that 2 mmol of 3,4-O-isopropylidene pyridoxine is added,the dosage of Ni2MgGa hydrotalcite catalyst is 1.0 g,8 mL mesitylene is used as solvent,the flow rate of oxygen is 10 mL·min-1,reaction temperature remains at 110℃,and the reaction has performed for 6 h.This study tries to provide an economic and green method for the synthesis of 3,4-O-isopropylidene pyridoxal.