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    • 8. 发明授权
    • Continuous preparation of phosphoric acid alkyl ester dichlorides
    • 连续制备磷酸烷基酯二氯化物
    • US4296047A
    • 1981-10-20
    • US129852
    • 1980-03-12
    • Karl-Julius SchmidtFriedrich SchmidtPeter SiegleGert Hansen
    • Karl-Julius SchmidtFriedrich SchmidtPeter SiegleGert Hansen
    • C07F9/12C07F9/14
    • C07F9/14
    • In the preparation of a phosphoric acid alkyl ester dichloride by reacting phosphorus oxychloride with an aliphatic alcohol according to the equation ##STR1## in which R represents C.sub.1 -C.sub.5 -alkyl,the improvement which comprises carrying out the reaction continuously at a temperature of about 10.degree. to 50.degree. C. using an excess of phosphorus oxychloride of about 5 to 40%. The excess phosphorus oxychloride is reacted with the alcohol by continuous mixing, the reaction mixture is cooled, substantially all the hydrogen chloride formed is then separated off in a preliminary degassing stage, the reaction mixture is worked up in a distillation column, the unreacted phosphorus oxychloride and any diluent is separated off over the top and condensed, the condensate is recycled to the reaction and the corresponding alkyl ester dichloride is removed continuously as the bottom product.
    • 在通过磷酰氯与脂肪醇反应制备磷酸烷基酯二氯化物时,其中R表示C1-C5-烷基,其中包括在约10℃的温度下连续进行反应的改进 使用过量的氯氧化磷,约5至40%。 过量的三氯氧磷通过连续混合与醇反应,将反应混合物冷却,然后在预脱气阶段将形成的所有氯化氢基本上分离出来,将反应混合物在蒸馏塔中处理,未反应的三氯氧磷 并且任何稀释剂在顶部分离并冷凝,将冷凝物再循环到反应中,并且相应的烷基酯二氯化物作为底部产物连续地除去。
    • 10. 发明授权
    • N-substituted .beta.-aminocrotonic acid esters
    • US4027037A
    • 1977-05-31
    • US557698
    • 1975-03-12
    • Peter SiegleKlaus SassePeter Rossler
    • Peter SiegleKlaus SassePeter Rossler
    • A01N37/44A01N43/46C07C67/00C07C227/08C07C229/30C07C313/00C07C323/17C07C323/25C07C323/30C07D223/04C07D295/145C07C101/28A01N9/20
    • C07D295/145A01N37/44
    • N-substituted .beta.-aminocrotonic acid esters of the formula ##STR1## in which R.sup.1 is hydrogen, or alkyl or alkenyl with up to 4 carbon atoms;R.sup.2 is straight-chain or branched alkyl or alkenyl with up to 9 carbon atoms, optionally interrupted by O or S, and optionally substituted by halogen, phenoxy, dimethylamino, cyclic alkyl or alkenyl with up to 8 carbon atoms which are optionally substituted by halogen, dimethylamino, or alkyl, alkoxy or alkylthio with up to 4 carbon atoms, phenyl which is optionally substituted by halogen, dimethylamino, phenoxy, or alkyl, alkenyl, acyl, alkoxy, alkenoxy or alkynoxy containing up to 4 carbon atoms, or a 5- or 6-membered heterocyclic ring containing at least one O, S or N hetero-atom and optionally substituted by halogen, alkyl or alkoxy containing up to 4 carbon atoms or R.sub.2 is further more cyclic alkyl or alkenyl with up to 8 carbon atoms optionally substituted by halogen, dimethylamino, or alkyl, alkoxy or alkylthio with up to 4 carbon atoms; phenyl optionally substituted by halogen, dimethylamino, phenoxy, or alkyl, alkenyl, acyl, alkoxy, alkenoxy or alkynoxy containing up to 4 carbon atoms; or a 5- or 6-membered heterocyclic ring containing at least one O, S or N heteroatom and optionally substituted by halogen, or alkyl or alkoxy containing up to 4 carbon atoms; orR.sup.1 and R.sup.2 together with the adjoining nitrogen atom form a heterocyclic structure optionally substituted by lower alkyl with 1-4 carbon atoms and optionally containing further heteroatoms in addition to nitrogen, andR.sup.3 is straight-chain or branched alkyl, alkenyl or alkynyl each with up to 10 carbon atoms, or cyclic alkyl or alkenyl with up to 8 carbon atoms, optionally substituted by halogen, alkoxy or alkyl-thio containing up to 4 carbon atoms, phenyl, 3,4-methylenedioxyphenyl, cyclic alkyl or alkenyl with up to 8 carbon atoms; phenyl optionally substituted by dioxymethylene or alkyl, alkenyl, alkynyl, alkoxy, alkenoxy, alkynoxy or acyl containing up to 4 carbon atoms; or a heterocyclic ring containing up to 6 atoms of which at least one is O, N or S, which ring is optionally bonded via alkyl containing up to 4 carbon atoms,Which inhibit the metamorphosis of arthropods.