广州化工
廣州化工
엄주화공
GUANGZHOU CHEMICAL INDUSTRY AND TECHNOLOGY
2014年
11期
62-63,70
,共3页
异噁唑%1′,3-联吡咯-2-羧酸乙酯%合成
異噁唑%1′,3-聯吡咯-2-羧痠乙酯%閤成
이오서%1′,3-련필각-2-최산을지%합성
isoxazole%ethyl 1H-[1′,3-bipyrrole] -2-carboxylate%synthesis
以异噁唑为原料,经碱性开环、亲核加成、成环脱羧、 Clauson-Kaas四步反应合成了1′,3-联吡咯-2-羧酸乙酯,其结构经1 H-NMR确认。由于本方法中异噁唑碱性开环与加成两步反应实现一锅法,并对脱羧成环及Clauson-Kaas反应条件进行了优化,简化了工艺操作,降低了分离难度,提高了收率和产品纯度,适用于公斤级生产。
以異噁唑為原料,經堿性開環、親覈加成、成環脫羧、 Clauson-Kaas四步反應閤成瞭1′,3-聯吡咯-2-羧痠乙酯,其結構經1 H-NMR確認。由于本方法中異噁唑堿性開環與加成兩步反應實現一鍋法,併對脫羧成環及Clauson-Kaas反應條件進行瞭優化,簡化瞭工藝操作,降低瞭分離難度,提高瞭收率和產品純度,適用于公斤級生產。
이이오서위원료,경감성개배、친핵가성、성배탈최、 Clauson-Kaas사보반응합성료1′,3-련필각-2-최산을지,기결구경1 H-NMR학인。유우본방법중이오서감성개배여가성량보반응실현일과법,병대탈최성배급Clauson-Kaas반응조건진행료우화,간화료공예조작,강저료분리난도,제고료수솔화산품순도,괄용우공근급생산。
1H-[1′,3 -bipyrrole] -2 -carboxylate was synthesized from isodaxale by employing four steps of reaction with base -catalyzed ring opening , nucleophilic addition , decarboxylation -cyclization and Clauson -Kaas reaction.Structure of the products was characterized by 1 H-NMR.Since base-catalyzed ring opening of isoxazole and the nucleophilic addition was achieved in a one -pot procedure , reaction conditions of decarboxylation -cyclization and Clauson-Kaas reaction were optimized , the synthetic and isolation process was simplified , and yield and purity were increased , which was suitable for large -scale production.