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    • 45. 发明授权
    • Preparation of 2,2-disubstituted 3-chloropropionic esters
    • 2,2-二取代的3-氯丙酸酯的制备
    • US4837357A
    • 1989-06-06
    • US111624
    • 1987-10-21
    • Franz MergerPeter Hettinger
    • Franz MergerPeter Hettinger
    • C07C67/03C07B61/00C07C67/307C07C67/44C07C69/63C07C69/65C07C69/675C07C69/708C07C69/732
    • C07C67/307C07C67/03C07C67/44
    • 2,2-Disubstituted 3-chloropropionic esters I ##STR1## where R.sup.1 and R.sup.2 are each C.sub.1 -C.sub.6 -alkyl, C.sub.2 -C.sub.6 -oxaalkyl, C.sub.2 -C.sub.6 -alkenyl, C.sub.2 -C.sub.6 -oxaalkenyl, aryl or C.sub.7 -C.sub.12 -aralkyl or R.sup.1 -C-R.sup.2 is 5-, 6- or 7-membered ring, R.sup.3 is C.sub.2 -C.sub.6 -oxaalkyl, C.sub.2 -C.sub.6 -alkenyl, C.sub.2 -C.sub.6 -oxaalkenyl or C.sub.7 -C.sub.12 -aralkyl, are prepared by converting 2,2-disubstituted 3-hydroxypropanals II ##STR2## into the esterdiol III ##STR3## reacting this esterdiol III in the presence of a transesterification catalyst with an alcohol R.sup.3 OH to give the 3-hydroxyester IV ##STR4## reacting the hydroxyester IV with a stoichiometric or greater than stoichiometric amount of the thionyl chloride and thermally decomposing the product to give the chloropropionic ester I.
    • 2,2-二取代的3-氯丙酸酯I,其中R 1和R 2各自是C 1 -C 6 - 烷基,C 2 -C 6 - 氧杂烷基,C 2 -C 6 - 烯基,C 2 -C 6 - 氧杂链烯基,芳基或C 7 -C 12 - 芳烷基或R1-C-R2是5-,6-或7-元环,R3是C2-C6-氧杂烷基,C2-C6-烯基,C2-C6-氧杂链烯基或C7-C12-芳烷基,是通过将2 将2-二取代的3-羟基丙醛II转化成酯二醇III在酯交换催化剂与醇R 3 OH的存在下使该酯二醇III反应,得到3-羟基酯IV使羟基酯IV 化学计量或大于化学计量的亚硫酰氯,并热分解产物得到氯丙酸酯I.
    • 48. 发明授权
    • Multiple-step process for the preparation of hexamethylene
diisocyanate-1,6 and/or isomeric aliphatic diisocyanates with six
carbon atoms in the alkylene residue
    • 用于制备在亚烷基残基中具有6个碳原子的六亚甲基二异氰酸酯-1,6-和/或异构脂族二异氰酸酯的多步法
    • US4596678A
    • 1986-06-24
    • US600143
    • 1984-04-13
    • Franz MergerFriedrich TowaeHans HellbachGunther IsbarnWaldemar Koehler
    • Franz MergerFriedrich TowaeHans HellbachGunther IsbarnWaldemar Koehler
    • C07C265/14C07C67/00C07C69/00C07C241/00C07C263/04C07C263/06C07C265/04
    • C07C263/04
    • Hexamethylene diisocyanate and/or isomeric alkylene diisocyanates having 6 carbon atoms in the alkylene radical, preferably 2-methylpentamethylene 1,5-diisocyanate and/or 2-ethyltetramethylene 1,4-diisocyanate are prepared without the use of phosgene in a multiple-step process by means of(a) reacting hexamethylene 1,6-diamine and/or isomeric alkylene diamines having 6 carbon atoms in the alkylene radical with urea and alcohol in the presence of dialkyl carbonate and/or carbamic acid alkyl ester as well as, in some cases, catalysts to form hexamethylene 1,6-dialkylurethane and/or isomeric alkylene dialkylurethanes having 6 carbon atoms in the alkylene radical,(b) separation and return to reaction step (a) of alcohol, dialkyl carbonate, and/or carbamic acid alkyl ester from the reaction mixture(c) evaporation of the hexamethylene 1,6-dialkylurethane and/or isomeric alkylene dialkylurethanes having 6 carbon atoms in the alkylene radical,(d) cleavage of the vaporized diurethanes into hexamethylene diisocyanate and/or isomeric alkylene diisocyanate having 6 carbon atoms in the alkylene radical and alcohol, and(e) fractional condensation of the cleavage products.
    • 在多步法中不使用光气制备在亚烷基中具有6个碳原子的六亚甲基二异氰酸酯和/或异构亚烷基二异氰酸酯,优选2-甲基五亚甲基-1,5-二异氰酸酯和/或2-乙基四亚甲基1,4-二异氰酸酯 通过(a)在碳酸二烷基酯和/或氨基甲酸烷基酯的存在下,使亚烷基中的六亚甲基1,6-二胺和/或具有6个碳原子的异构亚烷基二胺与脲和醇反应,以及在一些 情况下,在亚烷基中形成具有6个碳原子的六亚甲基1,6-二烷基氨基甲酸酯和/或异构亚烷基二烷基氨基甲酸酯的催化剂,(b)分离并返回到醇,碳酸二烷基酯和/或氨基甲酸烷基酯的反应步骤(a) (c)在亚烷基中蒸发具有6个碳原子的六亚甲基1,6-二烷基氨基甲酸酯和/或异构亚烷基二烷基氨基甲酸酯,(d)将汽化的二氨基甲酸酯裂解成h 亚烷基二异氰酸酯和/或亚烷基和醇中具有6个碳原子的异构亚烷基二异氰酸酯,和(e)裂解产物的分级缩合。