Process for the separation of enantiomers
    1.
    发明授权
    Process for the separation of enantiomers 失效
    分离对映异构体的方法

    公开(公告)号:US5641404A

    公开(公告)日:1997-06-24

    申请号:US596338

    申请日:1996-02-20

    IPC分类号: B01D15/08 C07B57/00

    摘要: A process for separating enantiomeric mixtures by liquid chromatography using a stationary phase that includes cellulose or amylose derivative and a mobile phase that includes methanol and pentane, the concentration of methanol in the mobile phase being greater than one tenth percent by volume and less than the saturation concentration of methanol in the mobile phase, the concentration of pentane being at least that necessary to resolve the enantiomeric mixture into its enantiomers with a resolution at least one and one half times greater than the pentane of the mobile phase is replaced with hexane.

    摘要翻译: PCT No.PCT / US94 / 09687 371日期1996年2月20日 102(e)日期1996年2月20日PCT 1994年8月25日PCT公布。 第WO95 / 05879号公报 日期1995年3月2日使用包含纤维素或直链淀粉衍生物的固定相和包含甲醇和戊烷的流动相通过液相色谱分离对映异构体混合物的方法,流动相中甲醇的浓度大于体积百分之十 并且小于流动相中甲醇的饱和浓度,所替代的戊烷浓度至少为将对映异构体混合物分解成其对映异构体所必需的浓度至少比流动相的戊烷高1.5倍。 用己烷。

    Asymmetric synthesis of .beta.-amino alcohols from chiral or achiral
enamines
    2.
    发明授权
    Asymmetric synthesis of .beta.-amino alcohols from chiral or achiral enamines 失效
    手性或非手性烯胺对β-氨基醇的不对称合成

    公开(公告)号:US5367073A

    公开(公告)日:1994-11-22

    申请号:US138613

    申请日:1993-10-15

    摘要: The present invention relates to a process for the synthesis of chiral enantiomerically pure .beta.-amino alcohols which are extraordinarily important as therapeutic agents for the treatment of a variety of human disorders and as chiral auxiliaries in organic synthesis. The hydroboration of enamines is a versatile and convenient method for the synthesis of both racemic and enantiomerically pure .beta.-amino alcohols in high yields. This methodology enables the synthesis of virtually any .beta.-amino alcohol. Hydroboration of these enamines with chiral organic borohydrides, e.g. either mono- or diisopinocampheylborane, followed by oxidation with aqueous or solid NaOH/30% H.sub.2 O.sub.2 or Me.sub.3 NO, gives the corresponding chiral .beta.-amino alcohol. Enantiomeric excesses ranged from 60% for reactions run at 25.degree. C. to greater than 99% for reactions run at -25.degree. C.

    摘要翻译: 本发明涉及合成手性对映异构纯的β-氨基醇的方法,其作为用于治疗多种人类疾病的治疗剂非常重要,并且作为有机合成中的手性助剂。 烯胺的硼氢化合物是以高产率合成外消旋和对映异构纯的β-氨基醇的通用和方便的方法。 该方法使得几乎可以合成任何β-氨基醇。 这些烯胺与手性有机硼氢化物的水解,例如 单或二蒎烷基硼烷,然后用水或固体NaOH / 30%H 2 O 2或Me 3 NO 3氧化,得到相应的手性β-氨基醇。 在25℃下进行的反应,对映异构体的过量范围为60%,对于在-25℃下进行的反应为大于99%

    1-(ARYLTHIO, ARYLSULFINYL AND ARYLSULFONYL)-1,1-DIHALOMETHANESULFONAMIDES
    6.
    发明授权
    1-(ARYLTHIO, ARYLSULFINYL AND ARYLSULFONYL)-1,1-DIHALOMETHANESULFONAMIDES 失效
    1-(ARYLTHIO,ARYLSULFINYL和ARYLSULFONYL)-1,1-二缩水甘油醚

    公开(公告)号:US3946007A

    公开(公告)日:1976-03-23

    申请号:US554953

    申请日:1975-03-03

    CPC分类号: C07D295/26 C07D211/10

    摘要: The compounds of the formula ##SPC1##In which R is lower alkyl, lower alkoxy or halo, x is an integer from 0 to 2, n is an integer from 0 to 3, Y is halo and R.sub.1 and R.sub.2 independently are hydrogen, lower alkyl, phenyl or substituted phenyl, or, together with the nitrogen atom, form a heterocyclic ring also containing up to one oxygen atom in the heterocycle. The compounds in which x is 0 are prepared by adding chlorine or bromine to a 1-arylthiomethanesulfonamide in the presence of pyridine to form the 1-arylthio-1, 1-dihalomethanesulfonamide. The compounds in which x is 1 or 2 is prepared by adding sodium hypochlorite or sodium hypobromite to a 1-(arylsulfinyl)methane-sulfonamide or a 1-(arylsulfonyl)methanesulfonamide to form the 1-(arylsulfinyl)-1,1-dihalomethanesulfonamide or 1-(arylsulfonyl)-1,1-dihalomethanesulfonamide, respectively. The compounds are useful as antimicrobial agents.

    摘要翻译: 式中R为低级烷基,低级烷氧基或卤素的化合物,x为0至2的整数,n为0至3的整数,Y为卤素,R 1和R 2各为氢,低级烷基,苯基 或取代的苯基,或者与氮原子一起形成在该杂环中也含有至多一个氧原子的杂环。 在吡啶存在下,通过在1-芳基硫代甲磺酰胺中加入氯或溴来制备x为0的化合物,形成1-芳硫基-1,1-二卤代甲磺酰胺。 通过向1-(芳基亚磺酰基)甲磺酰胺或1-(芳基磺酰基)甲磺酰胺中加入次氯酸钠或次溴酸钠,形成1-(芳基亚磺酰基)-1,1-二卤代甲磺酰胺制备x为1或2的化合物 或1-(芳基磺酰基)-1,1-二卤代甲磺酰胺。 这些化合物可用作抗微生物剂。

    N-(5,7-dibromo-1,3-benzoxathiol-2-ylidene)-N-methylmethanaminium
bromide, N-(5,7-diiodo-1,3-benzoxathiol-2-ylidene)-N-methylmethanaminium
iodide and their preparation
    10.
    发明授权
    N-(5,7-dibromo-1,3-benzoxathiol-2-ylidene)-N-methylmethanaminium bromide, N-(5,7-diiodo-1,3-benzoxathiol-2-ylidene)-N-methylmethanaminium iodide and their preparation 失效
    N-(5,7-二溴-1,3-苯并恶唑-2-亚基)-N-甲基甲基溴化铵,N-(5,7-二碘-1,3-苯并恶唑-2-亚基)-N-甲基甲胺碘化物和 他们的准备

    公开(公告)号:US4087445A

    公开(公告)日:1978-05-02

    申请号:US780889

    申请日:1977-03-24

    IPC分类号: C07D327/04 A61K31/40

    CPC分类号: C07D327/04 C07C323/00

    摘要: N-(5,7-Dibromo-1,3-benzoxathiol-2-ylidene)-N-methylmethanaminium bromide and the analogous diodo iodide, new compounds, are prepared by the thermal rearrangement of O-(2,4,6-tribromophenyl)-N,N-dimethylthiocarbamate and O-(2,4,6-triiodophenyl)-N,N-dimethylthiocarbamate. The first-named compound has antimicrobial utility. Both compounds are useful as starting materials for the preparation of bis-(3,5-dibromo-2-hydroxyphenyl)disulfide and 2,4-diiodo-6-mercaptophenol, respectively, by hydrolysis of the two first-named compounds with methanolic sodium hydroxide. Both the disulfide and the mercaptophenol compounds have antimicrobial utility.

    摘要翻译: 通过O-(2,4,6-三溴苯基)的热重排制备N-(5,7-二溴-1,3-苯并恶唑-2-亚基)-N-甲基甲铵溴化物和类似的二碘碘化物,新化合物 )-N,N-二甲基硫代氨基甲酸酯和O-(2,4,6-三碘苯基)-N,N-二甲基硫代氨基甲酸酯。 第一个命名的化合物具有抗菌效用。 两种化合物分别可用作制备双 - (3,5-二溴-2-羟基苯基)二硫化物和2,4-二碘-6-巯基苯酚的起始原料,通过两种首先命名的化合物与甲醇钠的水解 氢氧化物。 二硫化物和巯基苯酚化合物都具有抗菌效用。