X. Xin
2012
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Guangzhou Chemical Industry
Abstract
1-(3,5-Dimethoxyphenyl)-1-heptanone,an important intermediate for preparation of nabilone,was synthesized to form 3,5-Dimethoxybenzamide by cyanidation reaction and Grignard reaction.The better synthesis process conditions were that in cyanidation reaction: 0.2 moL 3,5-Dimethoxybenzamide as bench marks,adding time 2 h,w(NaOH)=50%,the solvent for chloroform,phase transfer catalyst for TEBA,the yield of 3,5-Dimethoxybenzamide was 74.39%,and in Grignard reaction: 0.25 moL 3,5-Dimethoxybenzonitrile as benchmark,Grignard reagent and 3,5-Dimethoxybenzonitrile molar ratio of 1.5:1,the backflow time for 12 h,the yield was 3,5-Dimethoxybenzonitrile was 92.1%.Two step total yield of 68.5%.The structures of the target product were confirmed by means of the boiling point and 1H NMR.