fNaOH.96Р4结论Р(1)3.乙硫基丁醛与乙酰乙酸甲酯进行的羟醛缩合反应所用的碱(氢氧化钠)与乙酰乙酸甲酯的摩尔比Р为2,0~2.5:l,反应顺利进行,而且收率高,几步总收率达89.6%.Р(2)目标化合物(I)的合成过程中,通过将无水甲醇加入到工业甲醇钠中,以降低其浓度,获得了较Р适宜的甲醇加入量,所得产品杂质少,纯度高.Р(3)本工艺反应条件温和,收率和成品纯度高,填补了国内生产工艺的空白,总收率(以乙酰乙酸甲Р酯为基准)可达76%,适于工业化生产.Р参考文献:Р【l】LIUChang-lingOtiJ长令)Creationofherbicidalcyclohexanedionederivatives(环己烯酮类除草剂的创制经纬)【JJ.ChineseJuornalРofPesticides(农药),2002.4l(6):46-46Р【2】JohnSandraJ,AllanR.prisingthesame【P】lРUSP:6300281.200l-l0-09.Р131TataoLuo,ELSobrante,Calif,elaLHerhic-idalsubstituted2-(I-(oxyamino)-alkylide-ne)-cyclohexane-I,3-diones【PI.USP:Р4440566,1984-04-03.Р【4】TataoL,WilliamL.Herbicidalcyclohexane-l,3-dionederivatives[P】.GB:2179352,1987-03-04,Р【5】bs,CharlesAllen(EastmanKodakCo.).Preparationof4-carboalkoxy-1,3?cyclohexanedionesaS,herbicideintermediates【P】lРEP:2331l7.1987-08-l9.
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