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    • 6. 发明授权
    • Process for preparing 9,11-unsaturated steroidal compound from the
corresponding saturated steroidal compound
    • 从相应的饱和甾族化合物制备9,11-不饱和甾族化合物的方法
    • US4328162A
    • 1982-05-04
    • US184552
    • 1980-09-05
    • John A. HyattCharles A. McCombs
    • John A. HyattCharles A. McCombs
    • C07J7/00C07J9/00C07J5/00
    • C07J9/00C07J7/004
    • The present invention provides a non-fermentation process for placing unsaturation at the 9,11 position in a steroidal compound. Also, the present invention provides a process whereby the modified steroidal compound can be separated from the reaction mixture without the use of chromatography. More specifically, the present invention provides a process whereby a steroid compound such as 17-.alpha.-hydroxy-progesterone is reacted to form the meta iodoaryl benzoate. The iodoarylbenzoate is then irradiated with visible light in the presence of an alkyl-m-iodobenzoate dichloride to form the 9.alpha.-chloro steroid derivative. The chlorinated steroid derivative can then be hydrolized to provide a 9.alpha.-chloro steroidal alcohol and m-iodobenzoic acid. The m-iodobenzoic acid is extracted by the use of an aqueous base. The chlorinated steroidal alcohol can then be recovered and converted by conventional dehalogenation techniques to steroidal unsaturated compound having a double bond in the 9,11 position of the steroid nucleus. Alternatively, the chlorinated steroid derivative can be dehalogenation and then hydrolized.
    • 本发明提供了在甾族化合物中在9,11位置放置不饱和度的非发酵方法。 此外,本发明提供了一种可以将经修饰的甾体化合物与反应混合物分离而不使用色谱法的方法。 更具体地,本发明提供了使类固醇化合物如17-α-羟基孕酮反应以形成间位碘代苯甲酸酯的方法。 然后在存在烷基 - 间碘苯甲酸二氯化物的情况下用可见光照射碘代芳基苯甲酸酯,形成9α-氯类固醇衍生物。 然后将氯化类固醇衍生物水解以提供9α-氯甾体醇和间碘苯甲酸。 间 - 碘苯甲酸用碱水溶液萃取。 然后可以通过常规脱卤技术回收氯化甾族醇并将其转化为在类固醇核的9,11位具有双键的甾体不饱和化合物。 或者,氯化类固醇衍生物可以是脱卤,然后水解。
    • 10. 发明授权
    • Water-dispersible or water-soluble D-tocotrienol compounds and methods
for making therefor
    • 水分散性或水溶性D-生育三烯酚化合物及其制备方法
    • US5869704A
    • 1999-02-09
    • US138785
    • 1998-08-24
    • John A. Hyatt
    • John A. Hyatt
    • C07B53/00C07B61/00C07D311/72C08G65/332
    • C07D311/72
    • The invention relates to a water-dispersible or water-soluble compound having the structure I ##STR1## wherein, R.sup.1,R.sup.2, and R.sup.3 are, independently, hydrogen or methyl, and R.sup.4 is--(CH.sub.2 CH.sub.2 O).sub.n CH.sub.2 CH.sub.2 OH, wherein n is from 10 to 100, wherein compound I is the substantially pure D-enantiomer. The invention further relates to a water-dispersible or water-soluble compound having the structure II ##STR2## wherein, R.sup.1, R.sup.2, and R.sup.3 are, independently, hydrogen or methyl, or the salt thereof, wherein compound II is the substantially pure D-enantiomer. The invention further relates to methods for making the tocotrienol compounds of the present invention.
    • 本发明涉及具有结构式I的水分散性或水溶性化合物,其中R1,R2和R3独立地为氢或甲基,R4为 - (CH2CH2O)nCH2CH2OH,其中n为 10至100,其中化合物I是基本上纯的D-对映异构体。 本发明还涉及具有结构II II的水分散性或水溶性化合物,其中R1,R2和R3独立地是氢或甲基,或其盐,其中化合物II是基本上纯的 D-对映异构体。 本发明还涉及制备本发明的生育三烯酚化合物的方法。