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公开(公告)号：US20220162189A1
公开(公告)日：2022-05-26
申请号：US17430794
申请日：2020-02-18
发明人： Wenxiang ZHOU , Wenfeng HUANG , Jiaxing HU
IPC分类号： C07D403/06
摘要： Disclosed is a method for preparing voriconazole and an intermediate thereof In the method, a voriconazole condensate isomer is reacted as a starting material in the presence of an acid to obtain 4-chloro-6-ethyl-5-fluoropyrimidine and 2′,4′-difluoro-2-[1-(1H-1,2,4-triazolyl)]acetophenone. A method for preparing voriconazole by using the intermediate thus obtained is further disclosed. By adopting the method of the present invention, the utilization rate of starting materials and auxiliary materials for preparing voriconazole on the basis of the prior art can be greatly improved, thereby reducing costs.
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公开(公告)号：US20240300911A1
公开(公告)日：2024-09-12
申请号：US18261480
申请日：2022-01-10
发明人： Jian ZHANG , Jichao WANG , Zheng HAN , Yihong XU , Jiaxing HU , Wenfeng HUANG , Yongjun JIN
IPC分类号： C07D307/81
CPC分类号： C07D307/81
摘要： The present invention provides a purification method for citalopram or S-citalopram or salts thereof, comprising the following steps: using a washing solution to treat a solution consisting of citalopram and a water-immiscible organic solvent and carrying out separation to obtain an organic layer containing citalopram, or using a washing solution to treat a solution consisting of S-citalopram and a water-immiscible organic solvent and carrying out separation to obtain an organic layer containing S-citalopram; and then, taking the organic layer and carrying out further separation to obtain citalopram or S-citalopram, or adding acid to form a salt and carrying out further separation to obtain an acid salt of citalopram or S-citalopram. The purification method provided by the present invention is simple in operation and high in impurity removal rate.
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公开(公告)号：US20240092729A1
公开(公告)日：2024-03-21
申请号：US18261363
申请日：2021-12-28
发明人： Jian ZHANG , Jichao WANG , Xiangqian YOU , Liangwei QIAN , Tao ZHOU , Jiaxing HU , Wenfeng HUANG
IPC分类号： C07C255/59 , C07C253/34
CPC分类号： C07C255/59 , C07C253/34
摘要： The present invention relates to a method for purifying key intermediates of Citalopram, i.e. 4-[4-(dimethylamino)-1-(4-fluorophenyl)-1-hydroxybutyl]-3-hydroxymethylbenzonitrile and a salt thereof. The method comprises dissolving crude 4-[4-(dimethylamino)-1-(4-fluorophenyl)-1-hydroxybutyl]-3-hydroxymethylbenzonitrile (compound of formula I containing formaldehyde impurity) with an organic solvent, adding a washing solution, controlling the temperature, stirring, leaving to stand for layering, and removing the aqueous layer, so as to obtain a purified organic solution of 4-[4-(dimethylamino)-1-(4-fluorophenyl)-1-hydroxybutyl]-3-hydroxymethylbenzonitrile. The method provided by the present invention can effectively remove aldehyde group-containing impurities in the intermediate. The method of the present invention has the advantages of simple operation, cheap raw materials and mild conditions, and is suitable for large-scale industrial production.
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公开(公告)号：US10961194B2
公开(公告)日：2021-03-30
申请号：US16623085
申请日：2017-06-16
发明人： Guoliang Tu , Zhongming Xu , Tao Zhou , Wenfeng Huang , Shiwen Zhang
IPC分类号： C07D209/34
摘要： Provided is a method for purifying ropinirole hydrochloride (4-2-di-n-propylaminoethyl-1,3-dihydro-2H-indole-2-ketohydrochloride). The method comprises: adding ropinirole hydrochloride containing a monopropyl impurity A into water, adding organic solvent, stirring and dissolving at room temperature, adding alkali, stirring, standing, demixing, and removing an aqueous layer; optionally, drying the organic layer by using anhydrous magnesium sulfate, and filtering; and adding acyl chloride or acid anhydride into the organic layer, stirring, concentrating the organic layer to be dry, adding an organic solvent into the obtained oily matter, adding concentrated hydrochloric acid, and stirring, so as to obtain the ropinirole hydrochloride. By using the method, the impurity A in the ropinirole hydrochloride can be effectively removed, and the ropinirole hydrochloride can be obtained with a high yield and a high purity, so that the impurity A is controlled and the purity of the product reaches a medicinal standard.
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公开(公告)号：US20200172482A1
公开(公告)日：2020-06-04
申请号：US16623085
申请日：2017-06-16
发明人： Guoliang TU , Zhongming XU , Tao ZHOU , Wenfeng HUANG , Shiwen ZHANG
IPC分类号： C07D209/34
摘要： Provided is a method for purifying ropinirole hydrochloride (4-2-di-n-propylaminoethyl-1,3-dihydro-2H-indole-2-ketohydrochloride). The method comprises: adding ropinirole hydrochloride containing a monopropyl impurity A into water, adding organic solvent, stirring and dissolving at room temperature, adding alkali, stirring, standing, demixing, and removing an aqueous layer; optionally, drying the organic layer by using anhydrous magnesium sulfate, and filtering; and adding acyl chloride or acid anhydride into the organic layer, stirring, concentrating the organic layer to be dry, adding an organic solvent into the obtained oily matter, adding concentrated hydrochloric acid, and stirring, so as to obtain the ropinirole hydrochloride. By using the method, the impurity A in the ropinirole hydrochloride can be effectively removed, and the ropinirole hydrochloride can be obtained with a high yield and a high purity, so that the impurity A is controlled and the purity of the product reaches a medicinal standard.
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公开(公告)号：US10227293B2
公开(公告)日：2019-03-12
申请号：US15580517
申请日：2015-06-09
申请人： Zhejiang Huahai Pharmaceutical Co., Ltd , Zhejiang Huahai Licheng Pharmaceutical Co., Ltd , Zhejiang Huahai Jiancheng Pharmaceutical Co., Ltd
发明人： Zunjun Liang , Weifeng Xiao , Caihua Peng , Wenfeng Huang , Guoliang Tu
IPC分类号： C07C253/30 , C07C255/59 , C07B49/00 , C07F3/02
摘要： The present invention relates to a method for preparing a citalopram diol represented by formula IV, comprising the following steps: in the existence of an auxiliary reagent of metal salt, allowing 5-cyanophthalide to sequentially subjected to Grignard addition reactions with p-fluorophenyl magnesium halide and N, N-dimethylaminopropyl magnesium halide in an organic solvent; and after the reactions are completed, performing hydrolysis and separation to obtain citalopram diol represented by formula IV. In the present invention, by adding an auxiliary reagent of metal salt, the activity and the selectivity of the Grignard reactions are remarkably improved, and the reaction yield is obviously enhanced.
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