广州化工
廣州化工
엄주화공
GUANGZHOU CHEMICAL INDUSTRY AND TECHNOLOGY
2015年
12期
56-57,108
,共3页
(R)-2,2′-二甲基丙烯酰胺-1,1′-联萘%手性%合成
(R)-2,2′-二甲基丙烯酰胺-1,1′-聯萘%手性%閤成
(R)-2,2′-이갑기병희선알-1,1′-련내%수성%합성
(R)-2,2′-bis(methacrylamide)-1,1′-binaphthyl%chirality%synthesis
以2-萘酚和80%水合肼为起始原料,经3步反应合成了光学活性的2,2′-二胺-1,1′-联萘。在缚酸剂存在下,将所得光学活性的二胺与甲基丙烯酰氯反应制备得到目标产物(R)-2,2′-二甲基丙烯酰胺-1,1′-联萘。各步产物的结构经核磁分析得到确认。研究了水合肼与2-萘酚的投料比对中间体2-萘肼收率的影响,以及缚酸剂类别、反应温度对目标产物收率的影响,得到了一种适宜的合成工艺路线。
以2-萘酚和80%水閤肼為起始原料,經3步反應閤成瞭光學活性的2,2′-二胺-1,1′-聯萘。在縳痠劑存在下,將所得光學活性的二胺與甲基丙烯酰氯反應製備得到目標產物(R)-2,2′-二甲基丙烯酰胺-1,1′-聯萘。各步產物的結構經覈磁分析得到確認。研究瞭水閤肼與2-萘酚的投料比對中間體2-萘肼收率的影響,以及縳痠劑類彆、反應溫度對目標產物收率的影響,得到瞭一種適宜的閤成工藝路線。
이2-내분화80%수합정위기시원료,경3보반응합성료광학활성적2,2′-이알-1,1′-련내。재박산제존재하,장소득광학활성적이알여갑기병희선록반응제비득도목표산물(R)-2,2′-이갑기병희선알-1,1′-련내。각보산물적결구경핵자분석득도학인。연구료수합정여2-내분적투료비대중간체2-내정수솔적영향,이급박산제유별、반응온도대목표산물수솔적영향,득도료일충괄의적합성공예로선。
Optically active 2,2′-diamine-1,1′-binaphthyl was synthesized by three-step reactions using 2-naphthol and 80%hydrazine hydrate as raw materials.In the presence of acid binding agent , the resulted optically active diamine was reacted with methacryloyl chloride to give the target compound ( R ) -2, 2′-bis ( methacrylamide ) -1, 1′-binaphthyl.The structures of the products were identified by NMR.The effect of the feed ratio of hydrazine hydrate to 2-naphthol on the yield of 2-naphthylhydrazine , and the effect of the type of acid binding agent , reaction temperature on the yield of target compound were investigated , a suitable synthetic route was obtained.