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    • 1. 发明授权
    • Preparation of cyclic acetals of 3-formyl-2-butenyltriphenylphosphonium
chloride
    • 制备3-甲酰基-2-丁烯基三苯基氯化鏻的环状缩醛
    • US5344995A
    • 1994-09-06
    • US85903
    • 1993-07-06
    • Wolfgang KrauseJoachim PaustWalter DoblerHagen Jaedicke
    • Wolfgang KrauseJoachim PaustWalter DoblerHagen Jaedicke
    • C07F9/54C07D319/06C07F9/655C07C43/305C07C43/313
    • C07F9/6552C07D319/06
    • An improved process for preparing cyclic acetals of 3-formyl-2-butenyltriphenylphosphonium chloride by acetalization of 3-formyl-2-butenyl acetate with an aliphatic 1,3-diol, conversion of the resulting 4-acetoxy acetal into the corresponding 4-hydroxy acetal, Vilsmeier chlorination to give the corresponding 4-chloro acetal and subsequent reaction with triphenylphosphine entails carrying out the first 3 steps in an aliphatic or cycloaliphatic hydrocarbon or mixture of hydrocarbons with 6-8 carbons and the reaction with triphenylphosphine in an alkanol with 1-3 carbons and/or in aliphatic or cycloaliphatic hydrocarbon with 6-8 carbons or a corresponding mixture of hydrocarbons. The process is particularly advantageous when conversion of the 4-acetoxy acetal into the 4-hydroxy acetal is carried out with an aqueous alkali metal hydroxide solution in the presence of phase-transfer catalysts, and the first three, or all four, reaction stages are carried out in the same C.sub.6 -C.sub.8 -hydrocarbon.
    • 通过用脂肪族1,3-二醇缩醛化3-甲酰基-2-丁烯基乙酸酯与3-甲酰基-2-丁烯基三苯基氯化鏻的环状缩醛的改进方法,将得到的4-乙酰氧基缩醛转化为相应的4-羟基 缩醛,Vilsmeier氯化,得到相应的4-氯缩醛,随后与三苯基膦反应需要在脂族或脂环族烃或碳原子数为6〜8的混合物中进行前3个步骤,并与三苯基膦在链烷醇中与1- 3个碳原子和/或具有6-8个碳原子的脂族或脂环族烃或相应的烃混合物。 当在相转移催化剂存在下,用碱金属氢氧化物水溶液进行4-乙酰氧基缩醛转化为4-羟基缩醛时,该方法是特别有利的,而前三个或所有四个反应阶段是 在相同的C6-C8-烃中进行。