Process for obtaining pure L-leucine
    11.
    发明授权
    Process for obtaining pure L-leucine 失效
    获得纯L-亮氨酸的方法

    公开(公告)号:US4562152A

    公开(公告)日:1985-12-31

    申请号:US612802

    申请日:1984-05-22

    摘要: Pure L-leucine is obtained from an aminoacid mixture which contains at least 45 weight percent L-leucine, at most 40 weight percent L-isoleucine and at most 25 weight percent of other aminoacids by acetylating the mixture, precipitating the acetylation product by acidification, subjecting the acetylation product to a saponification by an L-aminoacid acylate until 30 to 95% of the N-acetyl-L-leucine employed is saponified and isolating the L-leucine from the saponification mixture.

    摘要翻译: 纯L-亮氨酸由含有至少45重量%L-亮氨酸,至多40重量%L-异亮氨酸和至多25重量%其它氨基酸的氨基酸混合物获得,通过乙酰化混合物,通过酸化沉淀乙酰化产物, 使乙酰化产物用L-氨基酸酰化物进行皂化,直到使用的N-乙酰基-L-亮氨酸的30-95%皂化并从皂化混合物中分离出L-亮氨酸。

    Process for the recovery of S-(carboxymethyl)-(R)-cysteine and
S-(carboxymethyl)-(S)-cysteine
    12.
    发明授权
    Process for the recovery of S-(carboxymethyl)-(R)-cysteine and S-(carboxymethyl)-(S)-cysteine 失效
    S-(羧甲基) - (R) - 半胱氨酸和S-(羧甲基) - (S) - 半胱氨酸的回收方法

    公开(公告)号:US4551548A

    公开(公告)日:1985-11-05

    申请号:US477514

    申请日:1983-03-21

    摘要: The subject matter of the invention is a process for the recovery of S-(carboxymethyl)-(R)-cysteine and S-(carboxymethyl)-(S)-cysteine from a mixture of the two enantiomers. The mixture to be separated is dissolved in water in the presence of sufficient ammonia that the ammonium salt solution formed has a pH between 6 and 9. Then there is brought about in the solution of ammonium salt a state of supersaturation by the addition of seeding crystals of the ammonium salt of one of the two enantiomers, insofar as the starting material contains one of the two enantiomers in excess, the ammonium salt of this enantiomer, the ammonium salt of one of the two enantiomers is brought to crystallization and separated off. Subsequently by addition of seeding crystals of the ammonium salt of the other enantiomers to the remaining mother liquor the ammonium salt of this enantiomer is likewise brought to crystallization and separated off. Finally the respective S-(carboxymethyl)-cysteine is set free from the two ammonium salts.

    摘要翻译: 本发明的主题是从两种对映异构体的混合物中回收S-(羧甲基) - (R) - 半胱氨酸和S-(羧甲基) - (S) - 半胱氨酸)的方法。 待分离的混合物在足够的氨存在下溶解在水中,形成的铵盐溶液的pH值在6和9之间。然后在铵盐溶液中引入过饱和状态,加入晶种 的两种对映异构体之一的铵盐,只要起始原料含有过量的两种对映异构体之一,该对映异构体的铵盐,两种对映异构体之一的铵盐结晶并分离出来。 随后通过将其它对映异构体的铵盐的晶体晶体加入到剩余的母液中,同时将该对映异构体的铵盐进行结晶并分离。 最后,将各自的S-(羧甲基) - 半胱氨酸设定为不含这两种铵盐。

    Process for the separation of the racemate (R,S)-cysteine
    14.
    发明授权
    Process for the separation of the racemate (R,S)-cysteine 失效
    分离外消旋物(R,S) - 半胱氨酸的方法

    公开(公告)号:US4430509A

    公开(公告)日:1984-02-07

    申请号:US460858

    申请日:1983-01-25

    CPC分类号: C07H15/14

    摘要: To separate the racemate (R,S)-cysteine, the racemate is condensed in an inert solvent with an enantiomerically enantiomeric monosaccharide of the group of aldoses having 4 to 7 carbon atoms to form the corresponding 2-substituted thiazolidin-4-carboxylic acid and the mixture of diastereomers obtained separated from each other. Subsequently, the isolated unitary diastereomers are reacted in an inert solvent with a carbonyl reagent to split the ring and the enantiomerically pure cysteine in each case is isolated as such or as the corresponding cystine.

    摘要翻译: 为了分离外消旋体(R,S) - 半胱氨酸,外消旋体在惰性溶剂中与具有4至7个碳原子的醛糖组的对映异构体对映异构体单糖缩合形成相应的2-取代的噻唑烷-4-羧酸, 获得的非对映异构体的混合物彼此分离。 随后,将分离的单一非对映异构体在惰性溶剂中与羰基试剂反应以分裂环,并且每种情况下的对映体纯的半胱氨酸本身或相应的胱氨酸分离。

    Thin-layer chromatographic method for the separation of enantiomers
    19.
    发明授权
    Thin-layer chromatographic method for the separation of enantiomers 失效
    用于分离对映异构体的薄层色谱法

    公开(公告)号:US4590167A

    公开(公告)日:1986-05-20

    申请号:US634685

    申请日:1984-07-25

    摘要: Thin-layer chromatography is employed to separate enantiomers of the general formula, ##STR1## in which C* represents an asymmetric center and the substituents R.sup.1, R.sup.2, and R.sup.3 are such that they supply the structural element ##STR2## for .alpha.-amino- or .alpha.-iminocarboxylic acids, particularly the well-known .alpha.-amino- or .alpha.-iminocarboxylic or for derivatives of such carboxylic acids, either of which contains no free thiol groups. In the thin-layer chromatographic separation operation a TLC plate is used which is coated with silica gel hydrophobicized by a silane derivative and which is further impregnated with an ionic compound of a divalent transition metal and a chiral selector. The mobile phase employed is a ternary mixture of a water-miscible alkanol, such as methanol, water, and acetonitrile, or a quaternary mixture of the latter ternary mixture to which a water-miscible cyclic ether, such as tetrahydrofuran, has been added.

    摘要翻译: 使用薄层色谱分离通式为“IMAGE”的对映异构体,其中C *表示不对称中心,并且取代基R 1,R 2和R 3使得它们提供α-氨基 - 或α-亚胺羧酸,特别是众所周知的α-氨基 - 或α-亚胺基羧酸或这些羧酸的衍生物,其中任一种不含游离巯基。 在薄层色谱分离操作中,使用TLC板,其上涂有用硅烷衍生物疏水化的硅胶,并进一步用二价过渡金属和手性选择剂的离子化合物浸渍。 使用的流动相是水混溶性链烷醇如甲醇,水和乙腈的三元混合物,或后者三元混合物的四元混合物,其中加入水混溶性环醚如四氢呋喃。

    Optically active proline derivative, process for its production and use
    20.
    发明授权
    Optically active proline derivative, process for its production and use 失效
    光学活性脯氨酸衍生物,其生产和使用过程

    公开(公告)号:US4469875A

    公开(公告)日:1984-09-04

    申请号:US426132

    申请日:1982-09-28

    摘要: The invention is directed to optically active proline derivative of the general formula: ##STR1## in which X is a hydrogen atom or a hydroxyl group and R is a hydrogen atom, an unsubstituted or alkyl group substituted phenyl group or a straight chain or branched alkyl group having 1 to 20 carbon atoms and a process for its production by reacting an enantiomerically pure proline or 4-hydroxy-proline as a solution in an alkanol having 1 to 4 carbon atoms with 0.9 to 2 times the molar amount of an alkali metal alcoholate corresponding to the alkanol and 1 to 3 times the molar amount of an epoxide of the general formula ##STR2## in which R is as defined above. The optically active proline derivative of general formula (I) can be used in the form of metal ion chelate complexes as the chiral stationary phase in the separation of enantiomers by means of liquid chromatography.

    摘要翻译: 本发明涉及以下通式的光学活性脯氨酸衍生物:其中X为氢原子或羟基,R为氢原子,未取代或烷基取代的苯基或直链 或碳原子数为1〜20的支链烷基,其制造方法为使对映异构体纯的脯氨酸或4-羟基脯氨酸作为溶解于具有1〜4个碳原子的链烷醇中的溶液的0.9〜2倍 对应于链烷醇的碱金属醇化物和通式为其中R如上定义的通式为(II)的环氧化物的摩尔量的1至3倍。 通过液相色谱分离对映异构体,通式(I)的光学活性脯氨酸衍生物可以以金属离子螯合物的形式用作手性固定相。