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    • 11. 发明申请
    • PROCESS FOR CONTINUOUSLY PREPARING DI-C1-3-ALKYL SUCCINATES
    • 连续制备DI-C 3-烷基琥珀酸酯的方法
    • WO2014180871A1
    • 2014-11-13
    • PCT/EP2014/059278
    • 2014-05-07
    • BASF SE
    • DEMMING, StefanieTHOTLA, SumanWITTENBERG, JensIFFLAND, GabrieleBRÜGGEMANN, Till, ChristianHOELZL, YvonneSIEGEL, WolfgangFREYER, Stephan
    • C07C67/08
    • C07C67/08B01D3/141C07C67/54C07C69/40
    • The invention relates to a process for continuously preparing di-C 1-3 -alkyl succinates by reacting succinic acid with an C 1-3 -alkanol in the presence of a fixed-bed heterogeneous acidic esterification catalyst in a tubular reactor at a temperature in the range of from 60 to 100°C, wherein a mixture, comprising succinic acid, C 1-3 -alkanol, mono-C 1-3 -alkyl succinate, di-C 1-3 -alkyl succinate and water, is formed in a mixing stage and fed to the entrance of the tubular reactor, and wherein 5 to 75% of the outlet flow rate of the tubular reactor are recycled directly to the mixing stage as a recycle stream, and the molar ratio of C 1-3 -alkanol to succinic acid added to the mixing zone, and not including the C 1-3 -alkanol and succinic acid at the recycle stream, being in the range of from 2.0 to 9.5. The invention furthermore relates to a process for separating the reactor effluent of an esterification of succinic acid with an C 1-3 -alkanol to give di-C1-3-alkyl succinates by distillation, wherein the separation is performed in a divided wall column in which C 1-3 -alkanol and water are removed in a top draw of the column, di-C 1-3 -alkyl succinate is removed in a side draw of the column, and wherein mono-C 1-3 -alkyl succinate and succinic acid are removed in a bottom draw of the column.
    • 本发明涉及一种连续制备二-C1-烷基琥珀酸盐的方法,该方法是在固定床非均相酸性酯化催化剂存在下,在管式反应器中在一定温度范围内使琥珀酸与C 1-3烷醇反应 为60〜100℃,其中在混合阶段中形成包含琥珀酸,C 1-3链烷醇,琥珀酸单C 1-3烷基酯,琥珀酸二-C 1-3烷基酯和水的混合物,并加入 到管式反应器的入口,并且其中管式反应器的出口流量的5%至75%作为循环流直接循环到混合阶段,并且将C 1-3烷醇与琥珀酸的摩尔比加到 混合区,并且在再循环流中不包括C 1-3烷醇和琥珀酸,其范围为2.0-9.5。 本发明还涉及一种将琥珀酸酯化为C 3-链烷醇的反应器流出物分离以通过蒸馏得到二-C1-烷基琥珀酸酯的方法,其中分离是在分隔壁塔中进行的,其中在 在柱的顶部萃取中除去C 1-3链烷醇和水,在柱的侧馏分中除去琥珀酸二-C1--3烷基酯,并且其中除去C 1 -C 3烷基琥珀酸酯和琥珀酸单 在列的底部绘制。
    • 18. 发明申请
    • PROCESS FOR PREPARING OF CAROTENOID MONO-ESTERS
    • 制备类胡萝卜素单酯的方法
    • WO2018050794A1
    • 2018-03-22
    • PCT/EP2017/073220
    • 2017-09-15
    • BASF SE
    • SCHAEFER, BerndSIEGEL, Wolfgang
    • C07C403/24
    • C07C403/24C07C2601/16
    • The present invention relates to a process for preparing a carotenoid mono-ester of the formula (I), including the stereoisomers of formula (I), wherein, R 1 is e.g. hydrogen, C 1 -C 20 -alkyl, C 2 -C 20 -alkenyl, C 4 -C 20 -alkdienyl, C 6 -C 20 -alktrienyl or C 8 -C 20 -alktetraenyl, R 2 is e.g. hydrogen or -NR a R b , wherein R a is e.g. hydrogen, C 1 -C 4 -alkyl, -C(O)-C 1 -C 3 -alkyl, -Boc or -Cbz, R b is e.g. hydrogen or C 1 -C 4 -alkyl, R 3 is e.g. hydrogen, X 1 , X 2 are independently from each other CH 2 or C=O, which comprises reacting a phosphonium salt of the formula (II) or a stereoisomer thereof: wherein X 1 , R 1 , R 2 , and R 3 are as defined for formula (I), R 4 is phenyl, tert-butyl or tolyl, and Y - is a suitable counteranion, with a 12'-apocarothenal of the formula (III) or a stereoisomer thereof: wherein X 2 is as defined for formula (I), in the presence of a base or a cryptobase.
    • 本发明涉及制备式(I)的类胡萝卜素单酯的方法,包括式(I)的立体异构体,其中R 1为 例如 氢,C 1 -C 20 - 烷基,C 2 -C 20 - 烯基,C 1 -C 20烷基, 4-C 20 - 链二烯基,C 6 -C 20 - 烷叉基或C 8 - 例如C 20 - 四链烯基,R 2是例如 氢或-NR a R b,其中R a是例如甲基,乙基,丙基,异丙基,丁基等。 氢,C 1 -C 4 - 烷基,-C(O)-C 1 -C 3 - , - C 1 -C 4 - 烷基,-Boc或-Cbz,R b是例如 氢或C 1 -C 4 - 烷基,R 3是例如C 1 -C 4烷基。 氢,X 1,X 2彼此独立地为CH 2或C = O,该方法包括使式(ⅩⅩ)的鏻盐与式 II)化合物或其立体异构体:其中X 1,R 1,R 2和R 3如上所述 对于式(I)定义的R 4是苯基,叔丁基或甲苯基,Y 1是合适的抗衡阴离子,与式(I)的12'-对氨基苯甲醛 III)或其立体异构体:其中X 2如式(I)中所定义,在碱或隐窝碱存在下进行。
    • 19. 发明申请
    • PROCESS FOR PREPARING PHOSPHONIUM SALT ESTERS AS BUILDING BLOCKS FOR CAROTENOIDES
    • 用于制备类胡萝卜素块的磷鎓盐酯的方法
    • WO2018050793A1
    • 2018-03-22
    • PCT/EP2017/073219
    • 2017-09-15
    • BASF SE
    • SCHAEFER, BerndSIEGEL, Wolfgang
    • C07F9/54C07C403/08C07C403/16C07C403/24
    • C07F9/5442
    • The present invention relates to a process for preparing a phosphonium salt ester of the formula (I), wherein R 1 is e.g. hydrogen, C 1 -C 20 -alkyl, C 2 -C 20 -alkenyl, C 4 -C 20 -alkdienyl, C 6 -C 20 -alktrienyl or C 8 -C 20 -alktetraenyl, R 2 is e.g. hydrogen or -NR a R b , wherein R a is e.g. hydrogen, C 1 -C 4 -alkyl, -C(O)-C 1 -C 3 -alkyl, -Boc or -Cbz, R b is e.g. hydrogen or C 1 -C 4 -alkyl, R 3 is e.g. hydrogen, X is CH 2 or C=O, R 4 is phenyl, tert-butyl or tolyl, Y - is a suitable counteranion, the process being characterized in that an alcohol of the formula (IV), is reacted with a carboxylic acid or one of its derivatives of the formula (V), wherein the variables R 1 , R 2 and R 3 are as defined above, and for n = 1 the variable Z is halogen, -OH or -O-C(O)-C 1 -C 4 -alkyl, and for n = 2 the variable Z is O or S, wherein the reaction is carried out in the presence of a tertiary amine and in case a compound of the formula (IV) with Z = -OH is used also in the presence of an activator. The invention further relates to certain phosphonium salt esters of the formula (I).
    • 制备式(I)的鏻盐酯的方法本发明涉及制备式(I)的鏻盐酯的方法,其中R 1为例如 氢,C 1 -C 20 - 烷基,C 2 -C 20 - 烯基,C 1 -C 20烷基, 4-C 20 - 链二烯基,C 6 -C 20 - 烷叉基或C 8 - 例如C 20 - 四链烯基,R 2是例如 氢或-NR a R b,其中R a是例如甲基,乙基,丙基,异丙基,丁基等。 氢,C 1 -C 4 - 烷基,-C(O)-C 1 -C 3 - , - C 1 -C 4 - 烷基,-Boc或-Cbz,R b是例如 氢或C 1 -C 4 - 烷基,R 3是例如C 1 -C 4烷基。 氢,X是CH 2或C = O,R 4是苯基,叔丁基或甲苯基,Y是合适的抗衡阴离子, 该方法的特征在于使式(IV)的醇与式(V)的羧酸或其衍生物之一反应,其中变量R 1,R 2, 2和R3如上所定义,并且对于n = 1,变量Z是卤素,-OH或-OC(O)-C1- C 1-4烷基,并且对于n = 2,变量Z是O或S,其中反应在叔胺存在下进行并且在式(IV)的化合物与 Z = -OH也用于活化剂的存在。 本发明进一步涉及式(I)的某些鏻盐酯。