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Identification and Synthesis of Trace Impurities in Four Chemical Drugs Such as Ondansetron

AddTime:2019-07-24

1. α-asarone has anti-platelet, hypolipidemic, sedative, analgesic, antispasmodic, anti-atherosclerosis and other pharmacological activities. Because α-asarone is extracted from natural plants, it is generally artificial. Synthetic, but generally accompanied by the formation of the toxic substance β-asarone, and the column separation cannot be performed due to the similar polarity of the two. We have designed a simple and practical synthetic route for the preparation of pure α-asarone brain, which has mild reaction conditions, simple operation, low toxicity and low load catalyst. 

The α- and β-asarone mixed with 43:57 (tested by GC) were reacted in ethyl acetate as solvent, room temperature and 0.1 mol% of I 2 as catalyst for 6 h, and then isomerized into α-asarone. After isomerization, the ratio of α- and β-asarone was 97:3, and the recrystallization yield was 89.9%. 

The structure of the three by-products was confirmed to confirm that the I 2 catalytic process belongs to the carbocation mechanism. 2. Synthesis of steroid hormone drugs. Steroid hormone drugs have strong anti-infective, anti-viral and anti-shock pharmacological effects, and are widely used in the treatment of rheumatism, cardiovascular diseases, cancer, skin diseases and the like. The synthetic raw materials for steroidal drugs are generally cholesterol, diosgenin, sisal saponin, and saponin. In this paper, steroidal drugs and their intermediates were synthesized from 16-dehydropregnenolone acetateas the starting material. The following work was done: (1) 16-dehydropregnenolone acetate as the starting material, after deuteration reaction, Beckmann Rearrangement reaction, hydrolysis reaction, Grignard reaction, Oppenauer oxidation (Wage's oxidation), methyleneation reaction and steroid C1, dehydrogenation at position 2 to synthesize exemestane, methionone and its intermediates, all synthetic The chemical structures of the compounds were confirmed by ~1H NMR and ~(13)C NMR spectra.


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