顺式-全氢异吲哚的合成工艺改进

目的:改进米格列奈关键中间体顺式-全氢异吲哚的合成工艺。方法:用顺式-六氢邻苯二甲酸酐和尿素反应,得到顺式-六氢邻苯二甲酰亚胺,再用四氢锂铝还原得到目标,然后成磷酸盐后进行分离、纯化。结果:合成得到目标产物的磷酸盐,产品纯度大于98%,两步反应的收率达到65%,结构经1HNMR和ESI-MS确证。结论:此工艺对产品纯化方法进行了改进,操作简单,提高了产品收率,储存方便,更适合于工业化生产的要求。

Improved Synthetics Technology of Cis-hexahydroisoindoline

Objective： Improved synthetics technology of cis-hexahydroisoindoline, an important intermediate of mitiglinide. Methods： Cis-hexahydrophthalic anhydride reacted with urea to obtain cis-hexahydrophthalimide, followed by reduction reaction with lithium-aluminum hydride to obtain target compounds, reacted with phosphoric acid to obtain phosphate, and then separated and purified after reaction. Results： The target compound was synthesized, its purity was more than 98 % and the total yield was 65 %, its structure was confirmed by IHNMR and ESI-MS. Conclusion： Improved Purification method of the target compounds, simplieation operation, improved yield of the target compounds, storing was easiest. The synthesis method was suitable for industry.