一种β-联苯双酯的改进制备方法  

Improved Preparation Method of β-DDB

作　　者：黄光东 石岳崚 何敏焕 陈明龙 穆晴晴 HUANG Guang-dong;SHI Yue-ling;HE Min-huan;CHEN Ming-long;MU Qing-qing(Zhejiang Hisoar Pharmaceutical Co.,Ltd.,Zhejiang Taizhou 318000,China)

机构地区：[1]浙江海翔药业股份有限公司

出　　处：《广州化工》2019年第23期65-67,共3页GuangZhou Chemical Industry

摘　　要：β-联苯双酯是合成五味子丙素及五味子酯丁的重要中间体。β-联苯双酯可通过两分子6-溴-3,4-亚甲二氧基-5-甲氧基苯甲酸甲酯经Ullmann偶合得到,其偶合单体的区域选择性6-位溴化成为大量制备β-联苯双酯的关键。本文通过选择性脱溴方法制备得到6-溴化物,进而制备得到β-联苯双酯。产物经IR,1HNMR,13 CNMR,1H-1H COSY,HSQC,HMBC和MS进行结构确认。本方法操作简单,原料价廉易得,适合于工业化大生产。β-DDB is an important intermediate for synthesis of Schisantherin C and Schisantherin D.β-DDB can be obtained by Ullmann coupling of two molecules of methyl 6-bromo-3,4-methylenedioxy-5-methoxybenzoate,and the regioselective 6-position bromination of the coupling monomer becomes the key to the large-scale preparation of β-DDB.6-bromide was prepared by selective debromination method,andβ-DDB was prepared.The structure of target compounds were confirmed by IR,1HNMR,13 CNMR,1H-1H COSY,HSQC,HMBC and MS.This method was simple and materials were cheap and available,suitable for large-scale industrial production.

关 键 词：β-联苯双酯 选择性脱溴 Ullmann偶合 

分 类 号：TQ463+.4[化学工程—制药化工]