Process for the preparation of an optically active ester
    6.
    发明公开
    Process for the preparation of an optically active ester 审中-公开
    韦尔法罕zur Herstellung eines optisch-aktiven Esters

    公开(公告)号:EP1710221A1

    公开(公告)日:2006-10-11

    申请号:EP05075828.3

    申请日:2005-04-07

    摘要: The invention relates to a process for the preparation of an optically active compound from raw materials comprising a di-ester and a chiral hydroxy-compound according to formula (I):

    wherein:
    - R 1 , R 2 , R 4 and R 5 each independently represent hydrogen or an alkyl group with 1-20 C-atoms, an alkenyl group with 2-20 C-atoms, an alkynyl group with 2-20 C-atoms,or an (hetero)aryl group with 4-20 C-atoms optionally containing one or more O, S or N atoms,
    - R 3 represents an alkyl group with 1-20 C-atoms, an alkenyl group with 2-20 C-atoms, an alkynyl group with 2-20 C-atoms, or an (hetero)aryl group with 4-20 C-atoms optionally containing one or more O, S or N atoms,
    - the compound according to formula (I) comprises at least one chiral centre that has an α-carbon relative to a secondary hydroxy group,

    comprising the steps of
    a) bringing the di-ester, optionally a solvent, and the chiral hydroxy-compound according to formula (I) together to form a reaction system;
    b) adding an asymmetric transesterification catalyst, a racemisation catalyst and optionally a racemisation catalyst re-activating compound to the reaction system;
    c) bringing the reaction system to conditions where racemisation and enantioselective transesterefication take place, whereby the optically active compound is formed,

    whereby steps a), b) and c) may be executed sequentially or simultaneously, and whereby the chiral hydroxy-compound according to formula (I) may in step a) be partially or wholly replaced by the combination of the corresponding ketone and a reducing agent.

    摘要翻译: 本发明涉及一种由包含二酯和根据式(I)的手性羟基化合物的原料制备光学活性化合物的方法:其中:-R 1,R 2,R 4和R 5各自为 独立地表示氢或具有1-20个C原子的烷基,具有2-20个C原子的烯基,具有2-20个C原子的炔基或具有4-20个C-原子的(杂)芳基, 任选地含有一个或多个O,S或N原子的原子,-R 3表示具有1-20个C原子的烷基,具有2-20个C原子的烯基,具有2-20个C原子的炔基, 或具有任选含有一个或多个O,S或N原子的4-20个C原子的(杂)芳基, - 根据式(I)的化合物包含至少一个手性中心,该手性中心相对于 仲羟基,包括以下步骤:a)将二酯,任选的溶剂和根据式(I)的手性羟基化合物一起制成反应体系; b)向反应体系中加入不对称酯交换催化剂,外消旋化催化剂和任选的外消旋催化剂再活化化合物; c)使反应体系进行进行外消旋化和对映选择性过渡发生的条件,从而形成光学活性化合物,由此可以顺序或同时进行步骤a),b)和c),由此根据 式(I)可以在步骤a)中被相应的酮和还原剂的组合部分或全部代替。

    PROCESS FOR CONTINUOUS PRODUCTION OF DIALKYL CARBONATE AND DIOL
    7.
    发明公开
    PROCESS FOR CONTINUOUS PRODUCTION OF DIALKYL CARBONATE AND DIOL 有权
    连续用于生产碳酸二烷基酯和DIALKYLDIOL

    公开(公告)号:EP1086940A4

    公开(公告)日:2004-04-07

    申请号:EP99923989

    申请日:1999-06-10

    摘要: A process comprising feeding continuously a cyclic carbonate and an aliphatic monohydric alcohol to a continuous multi-stage distillation column and forming (A) a dialkyl carbonate and (B) a diol, wherein a gaseous low boiling point mixture containing (A) is continuously withdrawn from the upper portion of the distillation column, while continuously withdrawing a liquid high boiling point mixture containing (B) from the lower portion of the distillation column, and a transesterification is carried out under a condition satisfying the following requirements (a) to (c): (a) 5 x 104 Pa or less in terms of the bottom pressure of the continuous multi-stage distillation column, (b) -20 °C to a temperature lower than 60 °C in terms of the bottom temperature of the continuous multi-stage distillation column, (c) 0.2 to 5.0 in terms of F-factor of the continuous multi-stage distillation column represented by the following formula (1): F-factor = u¿g? (ςg)?1/2¿ wherein u¿g? represents a gas flow rate in the continuous multi-stage distillation column (m/s), and ςg represents a gas density in the continuous multi-stage distillation column (kg/m?3¿).

    Process for producing benzyl alcohol
    8.
    发明公开
    Process for producing benzyl alcohol 失效
    Verfahren zur Herstellung von Benzylalkohol

    公开(公告)号:EP1164118A2

    公开(公告)日:2001-12-19

    申请号:EP01118520.4

    申请日:1996-12-03

    申请人: Tosoh Corporation

    IPC分类号: C07C29/09 C07C33/22

    摘要: According to the present application, a process is provided wherein benzyl acetate of high purity can be produced economically in one step reaction of oxyacetoxylation by constructing a distillation purification process in consideration of the boiling points, the solubilities, and the azeotropy of the components including benzyl acetate as an oxyacetoxylation product, unreacted toluene and acetic acid, and recycling the process distillation fractions to the specified process, by use of a specific catalyst composed of an alloy of palladium and bismuth supported on silica exhibiting high selectivity and has a long life of the catalyst.
    Furthermore, a process is provided wherein benzyl alcohol which cannot readily be isolated and purified from the hydrolysis product of benzyl acetate can be produced economically by constructing an isolation-purification process in consideration of the azeotropy of the components including benzyl alcohol and acetic acid as hydrolysis products, unreacted benzyl acetate and water, and recycling the process fractions to the specified process, and by using, as the catalyst, a sulfonated styrenedivinylbenzene copolymer having divinylbenzene units in a specified content range, and by reacting the starting materials in a specific ratio.
    Moreover, according to the present application, benzyl alcohol can be produced economically by transesterification of benzyl acetate with methanol in the presence of a basic catalyst, and combining process fractions reasonably in consideration of the later isolation-purification process.

    摘要翻译: 提供了一种方法,其中不能容易地从乙酸苄酯的水解产物中分离和纯化的苄醇可以通过考虑到包括苯甲醇和乙酸在内的成分的共沸作为水解产物构成分离纯化方法而经济地制备, 未反应的乙酸苄酯和水,并将工艺部分循环到指定的方法中,并且通过使用具有规定含量范围内的二乙烯基苯单元的磺化苯乙烯二乙烯基苯共聚物作为催化剂,并以特定比例使原料反应。 此外,根据本申请,可以在碱性催化剂存在下,通过乙酸苄酯与甲醇的酯交换,经济地生产苯甲醇,并考虑到后续的分离纯化方法合并工艺级分。

    VERFAHREN ZUR HERSTELLUNG VON POLYALKOHOLEN
    9.
    发明公开
    VERFAHREN ZUR HERSTELLUNG VON POLYALKOHOLEN 失效
    用于生产多元醇

    公开(公告)号:EP0876316A1

    公开(公告)日:1998-11-11

    申请号:EP96938170.0

    申请日:1996-11-11

    摘要: The invention relates to a process for the preparation of polyalcohols comprising the following stages: (a) reaction of an alcanal or ketone with formaldehyde in an aqueous solution in the presence of a tertiary amine; (b) separation of water, excess tertiary amine, excess formaldehyde; (c) heating of the remaining mixture of (b) separating further formaldehyde and tertiary amine and formation of polyalcohol formates; (d) conveying of tertiary amine separated from stage (b) and/ or stage (c) into the synthesis stage (a) and/or into the following transesterification stage (e); (e) transesterification of the polyalcohol formates obtained from stage (c) with an alcohol of the formula ROH in the presence of a transesterification catalyst to form polyalcohols and formates of the formula (I), R being a hydrocarbon radical, preferably an alkyl radical with 1-6, in particular preferably 1-2 C-atoms; (f) retrieval of polyalcohols.

    Process for producing tetrahydrofuran and 1,4-butanediol
    10.
    发明授权
    Process for producing tetrahydrofuran and 1,4-butanediol 失效
    生产四氢呋喃和1,4-丁二醇的方法

    公开(公告)号:EP0012376B1

    公开(公告)日:1982-04-21

    申请号:EP79104967.9

    申请日:1979-12-06

    摘要: A process for producing simultaneously tetrahydrofuran and 1,4-butanediol in any desired proportion which comprises (a) reacting the acetic ester of 1,4-butanediol with a theoretical or smaller quantity, based on said acetic ester, of water (preferably 0.2-0.8 mole of water per mole of said acetic ester) in the presence of an acidic catalyst, (b) distilling, in the first distillation column, the reaction mixture to separate it into a distillate comprising tetrahydrofuran as major constituent and a bottom stream comprising as major constituent the acetic ester of 1,4-butanediol and (c) subjecting, in the second reaction-distillation column, at least a part of said bottom stream to a counter-current gas-liquid contact reaction with methanol, the quantity of said methanol being preferably 1-5 moles per mole of the acetate group of the acetic ester, in the presence of an acidic or basic catalyst and, simultaneously therewith, separating the reaction mixture into a bottom stream comprising 1,4-butanediol as major constituent and a distillate comprising methyl acetate as major constituent. By this process, methanol and catalyst can be economized to a great extent.