CAJ | 학술논문

通过4-氯-5-环戊氧基-2-氟异氰酸苯酯与2 -羟基-3-甲基-3-丁烯腈发生加成环化反应制得除草剂3-(4-氯-5-环戊氧基-2- 氟苯基)-4-亚胺基-5-异丙叉基恶唑烷-2-酮。反应分两阶段进行，首先在冰水浴中向 2-羟基-3-甲基-3-丁烯腈中滴加4-氯-5-环戊氧基-2-氟异氰酸苯酯甲苯溶液，然后升至室温反应4 h。优化的反应条件为：三乙胺作催化剂，n(4-氯-5-环戊氧基-2 -氟异氰酸苯酯)∶n(2-羟基-3-甲基-3-丁烯腈)=1.0∶1.2，加料方式为滴加4 -氯-5-环戊氧基-2-氟异氰酸苯酯甲苯溶液，第二阶段反应在室温下进行。反应条件优化以后，产品收率可由39%提高到56%。产品结构用CIMS、1HNMR进行了确定。分离了其中一个副产物，并对其结构进行了鉴定。
통과4-록-5-배무양기-2-불이청산분지여2 -간기-3-갑기-3-정희정발생가성배화반응제득제초제3-(4-록-5-배무양기-2- 불분기)-4-아알기-5-이병차기악서완-2-동。반응분량계단진행，수선재빙수욕중향 2-간기-3-갑기-3-정희정중적가4-록-5-배무양기-2-불이청산분지갑분용액，연 후승지실온반응4 h。우화적반응조건위：삼을알작최화제，n(4-록-5-배무양기-2 -불이청산분지)∶n(2-간기-3-갑기-3-정희정)=1.0∶1.2，가료방식위적가4 -록-5-배무양기-2-불이청산분지갑분용액，제이계단반응재실온하진행。반응조건우 화이후，산품수솔가유39%제고도56%。산품결구용CIMS、1HNMR진행료학정。분리료기 중일개부산물，병대기결구진행료감정。
Herbicide 3-(4-chloro-5-cyclopentyloxy-2-fluorophen yl)-4-imine-5-isopropylideneoxazolidine-2-one(Ⅰ) is obtained through the addi tion cyclization of 4-chloro-5-cyclopentyloxy-2-fluorophenylisocyanate(Ⅱ) and 2-hydroxy-3-methyl-3-butenenitrile(Ⅲ).The reaction is carried out in two s teps.At first,under the cooling of ice-water mixture,the toluene solution cont aining Ⅱ is dropped into Ⅲ.Then the temperature is raised to room temper ature and the reaction proceeds for 4 h.Triethylamine is used as catalyst.Molar ratio of Ⅱ to Ⅲ is 1.0∶1.2.Under the above optimized conditions,yield of th e product(Ⅰ) can be raised from 39% to 56% .Structure of the product is confirmed by CIMS and 1 HNMR.A side-reaction product is separated,and its structure is identified.