摘要
联苯双酯在研究中药五味子过程中发现的一种新药,DDB中,单甲醚先环合后溴化,溴化收率仅有30%,五步总收率20%,本文选择单甲醚先溴化后环合,用溴化锌作催化剂,做L4(23)正交,得到合适工艺参数,催化剂溴化锌量为0.1 g,反应温度40℃,保温时间1 h,收率88%,含量98%以上,五步总收率30%,提高10%,其结构由红外、紫外、光谱、氢谱、质谱确认。
DDB was a new drug found in the study process of Chinese medicine Schisandra. In DDB, monomethyl ether first cyclization after bromide, the bromide yield was only 30%, and the five - step total yield was 20%. The monomethyl ether first bromided thengot cyclization, with zinc bromide as a catalyst to do L4 （2^3） orthogonal to obtain the appropriate process parameters. Under the conditons of content of zinc bromide O. 1 g, reaction temprature 40 ℃ and time 1 h,the yield was 88%, contain was more than 98%, five step total yield was 30%, and increased by 10%, and its structure was conformed by IR/UV/HNMR/MS.
出处
《广州化工》
CAS
2013年第7期104-106,共3页
GuangZhou Chemical Industry
关键词
联苯双酯
溴化
环合
DDB
bromination
cyclization
