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    • 5. 发明授权
    • Method for preparing D-biotin
    • D-生物素的制备方法
    • US09260449B2
    • 2016-02-16
    • US14483147
    • 2014-09-10
    • Zhejiang Medicine Co., Ltd., Xinchang Pharmaceutical Factory
    • Yajin PanShiqing PiWenzhen DingLixin GuAngfeng WeiYimin He
    • C07D495/04
    • C07D495/04
    • The invention discloses a D-biotin preparation method. In the prior art, with a synthesis method utilizing malonic acid diester as raw materials, impurities are also produced along with the obtained D-biotin. The D-biotin preparation method is characterized in that with the presence of dimethyl sulfoxide and inorganic base as catalysts, methane tricarboxylic acid trialkyl ester and (3aR, 8aS, 8bS)-1,3-dibenzyl-2-oxo-10H-iminazole [3,4-d] thiophene [1,2-a] sulfuryl halide are subjected to condensation reaction in methylbenzene solvent to obtain intermediate (3 aS,4S,6aR)-1,3-dibenzyl-4-(ω,ω,ω-3-methoxycarbonylbutyl)-4H-1H-thiophene[3,4-d]iminazol e-2,4(1H)-ketone, and the D-biotin is obtained after the intermediate is treated by the aftertreatment method. By the D-biotin preparation method, production of the impurities is avoided, quality of the biotin is greatly improved on the existing basis, and side reaction is avoided too.
    • 本发明公开了一种D-生物素的制备方法。 在现有技术中,利用以丙二酸二酯为原料的合成方法,与所得的D-生物素一起也产生杂质。 D-生物素制备方法的特征在于,在二甲基亚砜和无机碱作为催化剂的存在下,甲烷三羧酸三烷基酯和(3aR,8aS,8bS)-1,3-二苄基-2-氧代-10H-咪唑[ 3,4-d]噻吩[1,2-a]磺酰卤在甲苯溶剂中进行缩合反应,得到中间体(3 aS,4S,6aR)-1,3-二苄基-4-(ω,ω,ω -3-甲氧基羰基丁基)-4H-1H-噻吩[3,4-d]亚胺唑e-2,4(1H) - 酮,并且通过后处理方法处理中间体后得到D-生物素。 通过D-生物素制备方法,避免了杂质的生成,生物素的质量在现有的基础上大大提高,并且也避免副反应。