摘要
以5-甲基吡唑-3-甲酸甲酯和2-氰基苄溴为主要原料,经过N-烷基化取代反应、氢化铝锂还原反应、胺基保护反应以及氧化反应,得到了一种大环肽中间体—[2-(5-甲酰基-3-甲基-吡唑-1-甲基)-苄基]-氨基-9芴基甲酯,总摩尔收率为29.3%,各步所得产物经质谱、核磁共振氢谱等进行结构确证,其中第一步的N-烷基化取代反应,经过条件优化收率得到了提升至52.3%。
A compound of macrocyclic peptide intermediate-[2-(5-Formyl-3-methyl-pyrazol-1-ylmethyl)-benzyl]-carbamic acid 9H-fluoren-9-ylmethyl ester is synthesized through a series of reactions including alkylation substitution,reduction,amino protection and oxidation with 5-methylprazole-3-carboxylic acid methyl ester and 2-cyanobenzyl bromide as the main starting materials.The total molar yield is 29.3%,and the structures of all intermediate products are confirmed by MS and 1HNMR.The yield in the first-step alkylation substitution reaction is improved to 52.3%after process optimization.
作者
殷跃凡
龚晓莹
Yin Yuefan;Gong Xiaoying(Shanghai WuXi AppTec Co.,Ltd.,Shanghai 200131,China;Kunming Metallurgy College School of Architectural Engineering,Kunming 650300,China)
出处
《广东化工》
2026年第1期8-12,共5页
Guangdong Chemical Industry
