Research on Synthesis Technology of Ligustilide Dipolymer / 中国药房

ABSTRACT

OBJECTIVE:To study the synthesis technology of Ligustilide dipolymer (compound Ⅰ). METHODS:Using phthalic anhydride(compoundⅡ)as raw materials,sodium borohydride was reduced to phthalide(compound Ⅲ),and then syn-thesize ligustilide dipolymer after 4 steps. Ligustilide dipolymer was characterized by 1H-NMR and 13C-NMR. The synthesis technol-ogy of fifth step was optimized by orthogonal test with catalyzer,reaction temperature and reaction time as factors using yield as in-dex. The validation test was conducted. RESULTS:The optimal synthesis technology of fifth step was as follows as aluminium mu-riate of catalyzer,reaction temperature of 150 ℃,reaction time of 5 h. The average yield of validation test was 56.16%(RSD=1.23%,n=3). Total reaction yield was 24.4%,and the purity of target product was 99.4%. CONCLUSIONS:Ligustilide dipoly-mer is synthesized successfully;synthetic process is stable,and its quality is controllable.