4-Methylenepiperidine hydrochloride 1 is a key intermediate for synthesis of the novel antifungal
drug efinaconazole 2. In this work, a simple and robust process has been developed to synthesize
4-methylenepiperidine hydrochloride 1, with a high overall yield of 99.1% at a high purity of
99.7% in a large-scale. Moreover, this synthetic process avoided the uses of organolithium reagent and
column chromatography process which are not desirable for industrial production.
Zhongguo Yiyao Gongye Zazhi
Synthesis of Pregabalin
作者: Chen, Ao ; Zhang, Jianjun
The anticonvulsant pregabalin was synthesized using Me cyanoacetate as material by condensation, addition, cyclization, aminolysis, Hoffman rearrangement and resolution with (S)-mandelic acid.The overall yield of pregabalin was 16.1%.
The anticancer medicine imatinib mesylate was synthesized through condensation, reduction and cyclization reaction using 4-methyl-3-nitroaniline as raw material.The advantages of using anhydrous potassium carbonate instead of diisopropylethylamine, replacing Pt/C catalyst with hydrazine hydrate and common catalyst, using isopentyl alc. as solvent were discussed, resp.Finally, the total yield was over 50% and purity of product was over 99.5% identified by HPLC.
