Process of making D,L-lithium pantoate and resolving the racemic mixture
into its optically active isomers
    1.
    发明授权
    Process of making D,L-lithium pantoate and resolving the racemic mixture into its optically active isomers 失效
    制备D,L-锂泛酸盐并将外消旋混合物分解成其旋光异构体的方法

    公开(公告)号:US4115443A

    公开(公告)日:1978-09-19

    申请号:US670437

    申请日:1976-03-25

    IPC分类号: C07C59/105 C07C59/04

    CPC分类号: C07C59/105

    摘要: A process for the resolution of optical isomers of racemic lithium pantoate by selective crystallization from a solution in methanol, ethanol, or other polar solvents, or by electrostatic separation. The optical isomers can be readily converted to optically active pantolactones which are the starting material for the preparation of optically active pantothenic acid and its salt and pantothenyl alcohol. One of the two optical isomers of each of these compounds possesses vitamin activity. The unwanted or inactive optical isomer of lithium pantoate as such is thermally stable and can be racemized by heating in the presence of a basic reacting compound at a temperature between 120 and 180.degree. C to produce a racemic mixture which can then be subjected directly to resolution without conversion to some other derivative in accordance with the processes of the present invention to produce the desired or active optical isomer.

    摘要翻译: 通过从甲醇,乙醇或其它极性溶剂中的溶液中的选择性结晶或通过静电分离来拆分外消旋锂聚乙酸酯的光学异构体的方法。 光学异构体可以容易地转化为光学活性泛酸内酯,其是用于制备光学活性泛酸及其盐和泛氢苯醇的起始原料。 这些化合物中的每一种的两种光学异构体之一具有维生素活性。 锂泛酸锂的不需要的或不活泼的光学异构体本身是热稳定的,并且可以通过在120-180℃的温度下在碱性反应化合物的存在下加热进行外消旋化,以产生外消旋混合物,然后将其直接分解 而不根据本发明的方法转化成一些其它衍生物以产生所需或活性的旋光异构体。

    Lithium pantoate and optically active isomers thereof and process of
making the same
    2.
    发明授权
    Lithium pantoate and optically active isomers thereof and process of making the same 失效
    泛酸锂及其旋光异构体及其制备方法

    公开(公告)号:US4111987A

    公开(公告)日:1978-09-05

    申请号:US667411

    申请日:1976-03-16

    IPC分类号: C07C59/105 C07C59/04

    CPC分类号: C07C59/105

    摘要: A process for the resolution of optical isomers of racemic lithium pantoate by selective crystallization from a solution in methanol, ethanol, or other polar solvents, or by electrostatic separation. The optical isomers can be readily converted to optically active pantolactones which are the starting material for the preparation of optically active pantothenic acid and its salt and pantothenyl alcohol. One of the two optical isomers of each of these compounds possesses vitamin activity. The unwanted or inactive optical isomer of lithium pantoate as such is thermally stable and can be racemized by heating in the presence of a basic reacting compound at a temperature between 120.degree. and 180.degree. C to produce a racemic mixture which can then be subjected directly to resolution without conversion to some other derivative in accordance with the processes of the present invention to produce the desired or active optical isomer.

    摘要翻译: 通过从甲醇,乙醇或其它极性溶剂中的溶液中的选择性结晶或通过静电分离来拆分外消旋锂聚乙酸酯的光学异构体的方法。 光学异构体可以容易地转化为光学活性泛酸内酯,其是用于制备光学活性泛酸及其盐和泛氢苯醇的起始原料。 这些化合物中的每一种的两种光学异构体之一具有维生素活性。 锂泛酸锂的不需要的或不活泼的光学异构体是热稳定的,并且可以在碱性反应化合物存在下在120-180℃的温度下加热进行外消旋化,以产生外消旋混合物,然后将其直接进行 分辨率而不转化为根据本发明的方法产生所需或活性的光学异构体的一些其它衍生物。

    Process for making (DL) pantolactone
    4.
    发明授权
    Process for making (DL) pantolactone 失效
    制备(DL)泛酸内酯的方法

    公开(公告)号:US4124597A

    公开(公告)日:1978-11-07

    申请号:US667410

    申请日:1976-03-16

    IPC分类号: C07D307/33 C07D307/32

    CPC分类号: C07D307/33

    摘要: DL pantolactone is made by(a) introducing isobutyraldehyde, formalin and sodium cyanide solution continuously at a predetermined rate into a circulation reactor, continuously circulating the said mixture in said reactor while cooling the circulating mass in a heat exchanger, thus continuously causing the heat generated in the reaction between the components of said mixture to be discharged in said heat exchanger and by continuously re-mixing the formed reaction product with the reaction components;(b) continuously passing part of the reaction product into an after-treatment reactor where the said reaction is completed without re-mixing so as to form formisobutyraldolcyanohydrin;(c) passing the latter product into a first reaction chamber, reacting therein the product with a continuously introduced non-oxidizing strong acid at an elevated temperature and pressure so as to hydrolyze the product, thus forming a solution of .alpha.,.gamma.-dihydroxy-.beta.,.beta.-dimethylbutyric acid;(d) passing the said solution to a second reaction chamber and maintaining the solution therein at said elevated temperature and pressure until the .alpha.,.gamma.-dihydroxy-.beta.,.beta.-dimethylbutyric acid is lactonized to DL-.alpha.-hydroxy-.beta.,.beta.-dimethyl-.gamma.-butyrolactone and finally(e) recovering the latter product from the acid solution.The process permits obtaining DL-pantolactone in a continuous operation at a high yield.

    摘要翻译: DL泛酸内酯由(A)将丙三醇,甲醛和氰化钠溶液以预定的速率连续循环到循环反应器中,连续循环在热交换器中冷凝循环质量的同时反应器中的混合物,连续地引起热生成 在合格换热器中排放的混合物组分与反应组分连续重新混合形成的反应产物之间的反应中; (B)将反应产物的一部分连续通入反应器,在反应完成后,不再重新混合,从而形成甲基溴乙醇; (C)通过将产品输送到第一反应室,在产品的反应中连续引入非氧化强酸在高温和压力下进行水解,从而形成α,γ-二羟基 - β,β-二甲基丁酸; (D)将固体溶液通入第二反应室并维持其在高温和压力下的溶液,但α,γ-二羟基-β,β-二羟基丁酸被定义为DL-α-羟基-β,β- 二甲基γ-丁内酯,最后(E)从酸溶液中回收乳化剂产品。

    Apparatus for making (DL) pantolactone
    5.
    发明授权
    Apparatus for making (DL) pantolactone 失效
    制备(DL)泛酸内酯的装置

    公开(公告)号:US4095952A

    公开(公告)日:1978-06-20

    申请号:US733019

    申请日:1976-10-15

    IPC分类号: B01J19/24 C07D307/33 B01J1/00

    CPC分类号: C07D307/33 B01J19/2435

    摘要: An apparatus for making DL-pantolactone in a continuous process comprises the following parts and setup:A circulation heater and a circulation reactor, means for introducing the components into the reactor, a heat-exchanger forming part of the circulation reactor, a longitudinal aftertreatment reactor and a final longitudinal reactor comprising dual reaction chambers with means for applying heat and pressure in the first chamber and maintaining the reaction product in the second chamber at such heat and pressure. The apparatus may also include a chamber for forming a premix of some of the components with a subsequent cooling device prior to the introduction into the circulation reactor. It may furthermore include a stripping column and pulsation column for recovering the final product from the solution.

    摘要翻译: 在连续过程中制备DL-泛酸内酯的装置包括以下部分和设置: