文章摘要
胡旭,尹传奇.RDEA3170合成工艺优化[J].精细化工,2018,35(12):0
RDEA3170合成工艺优化
Synthetic process optimization of RDEA3170
投稿时间:2018-05-05  修订日期:2018-07-09
DOI:
中文关键词: 4-溴-1-萘甲腈  溴-镁交换反应  连续反应法  Suzuki偶联  RDEA3170  合成工艺优化
英文关键词: 4-bromo-1-naphthonitrile  bromo-magnesium exchanging reaction  continuous reaction method  Suzuki coupling  RDEA3170  synthetic process optimization
基金项目:湖北省教育厅重点项目(D20141510);湖北省教育厅项目(B2017053)
作者单位E-mail
胡旭 武汉工程大学 28203222@qq.com 
尹传奇 武汉工程大学 zhyfyin@126.com 
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中文摘要:
      利用1,4-二溴萘为起始原料,经溴-镁交换反应、4-溴-1-萘甲酰胺的合成和脱水,得到了一条新的4-溴-1-萘甲腈合成路线。通过连续反应法,以一种催化剂Pd(PPh3)2Cl2实现了4-溴-1-萘甲腈的Miyaura硼烷基化及其与2-((3-溴吡啶-4-基)硫)-2-甲基丙酸乙酯的Suzuki偶联。对偶联反应的最佳条件及产物水解生成RDEA3170的条件进行了优化。该合成路线RDEA3170的总收率达到42%,适合工业化生产。
英文摘要:
      4-bromo-1-naphthonitrile was obtained by a new route of bromo-magnesium exchanging reaction, synthesis and dehydration of 4-bromo-1-naphthamide using 1,4-dibromonaphthalene as starting materials. The Miyaura borylation of 4-bromine-1- naphthonitrile and its Suzuki coupling with ethyl 2-(3-bromopyridine-4-yl)thio-2-methylpropionate were realized using Pd(PPh3)2Cl2 as catalyst by a continuous reaction method. The conditions for coupling reaction and the hydrolysis of the product to produce RDEA3170 were optimized. The overall yield of RDEA3170 is 42% and the optimized synthetic process is suitable for the industrial production.
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