CN104744372A - 一种硝酸奥昔康唑的制备方法 - Google Patents

一种硝酸奥昔康唑的制备方法 Download PDF

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Publication number
CN104744372A
CN104744372A CN201310726742.8A CN201310726742A CN104744372A CN 104744372 A CN104744372 A CN 104744372A CN 201310726742 A CN201310726742 A CN 201310726742A CN 104744372 A CN104744372 A CN 104744372A
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oxiconazole nitrate
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蒋学京
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D233/00—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings
    • C07D233/54—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having two double bonds between ring members or between ring members and non-ring members
    • C07D233/56—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having two double bonds between ring members or between ring members and non-ring members with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, attached to ring carbon atoms
    • C07D233/61—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having two double bonds between ring members or between ring members and non-ring members with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, attached to ring carbon atoms with hydrocarbon radicals, substituted by nitrogen atoms not forming part of a nitro radical, attached to ring nitrogen atoms

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Plural Heterocyclic Compounds (AREA)

Abstract

本发明涉及一种硝酸奥昔康唑的制备方法，具体步骤如下：110.1g(1.62mol)咪唑悬浮于550mL二氯甲烷，在0～5℃和剧烈搅拌下，于约6h内加入120.5g(0.54mol)α，2，4-三氯苯乙酮溶于180mL二氯甲烷的溶液，加毕再搅拌1h，然后于室温下搅拌过夜。减压蒸去溶剂(低于40℃)，在剧烈搅拌下将剩余物溶于600mL水，过滤析出的沉淀，用水洗,得到的粗品可直接用于下步反应，如用甲醇重结晶，可得无色的化合物(Ⅰ)的结晶硝酸奥昔康唑。所述的一种硝酸奥昔康唑的制备方法，其制造过程简单，产量高，品质好。

Description

一种硝酸奥昔康唑的制备方法
技术领域
本发明涉及药物制备的领域，尤其是一种硝酸奥昔康唑的制备方法。
背景技术
硝酸奥昔康唑用于以下皮肤感染的局部治疗：红发癣菌、须发癣菌或絮状表皮癣菌所致的脚癣、股癣、体癣以及糠秕马拉色霉菌所致的花斑癣（糠疹）的局部治疗；还可用于儿童病人治疗体癣、股癣、脚癣和花斑癣（糠疹）。由于目前在于生产硝酸奥昔康唑中，制造过程复杂，生产成本高。
发明内容
本发明要解决的技术问题是：为了克服上述中存在的问题，提供了一种硝酸奥昔康唑的制备方法。
本发明解决其技术问题所采用的技术方案是：一种硝酸奥昔康唑的制备方法，具体步骤如下：110.1g(1.62mol)咪唑悬浮于550mL二氯甲烷，在0～5℃和剧烈搅拌下，于约6h内加入120.5g(0.54mol)α，2，4-三氯苯乙酮溶于180mL二氯甲烷的溶液，加毕再搅拌1h，然后于室温下搅拌过夜。减压蒸去溶剂(低于40℃)，在剧烈搅拌下将剩余物溶于600mL水，过滤析出的沉淀，用水洗,得到的粗品可直接用于下步反应，如用甲醇重结晶，可得无色的化合物(Ⅰ)的结晶硝酸奥昔康唑。
本发明的有益效果是：所述的一种硝酸奥昔康唑的制备方法，其制造过程简单，产量高，品质好。
具体实施方式
现在结合本发明作进一步详细的说明。
本发明的一种硝酸奥昔康唑的制备方法，具体步骤如下：110.1g(1.62mol)咪唑悬浮于550mL二氯甲烷，在0～5℃和剧烈搅拌下，于约6h内加入120.5g(0.54mol)α，2，4-三氯苯乙酮溶于180mL二氯甲烷的溶液，加毕再搅拌1h，然后于室温下搅拌过夜。减压蒸去溶剂(低于40℃)，在剧烈搅拌下将剩余物溶于600mL水，过滤析出的沉淀，用水洗,得到的粗品可直接用于下步反应，如用甲醇重结晶，可得无色的化合物(Ⅰ)的结晶硝酸奥昔康唑。
以上述依据本发明的理想实施例为启示，通过上述的说明内容，相关工作人员完全可以在不偏离本项发明技术思想的范围内，进行多样的变更以及修改。本项发明的技术性范围并不局限于说明书上的内容，必须要根据权利要求范围来确定其技术性范围。

Claims (1)

1.一种硝酸奥昔康唑的制备方法，其特征是具体步骤如下：110.1g(1.62mol)咪唑悬浮于550mL二氯甲烷，在0～5℃和剧烈搅拌下，于约6h内加入120.5g(0.54mol)α，2，4-三氯苯乙酮溶于180mL二氯甲烷的溶液，加毕再搅拌1h，然后于室温下搅拌过夜。减压蒸去溶剂(低于40℃)，在剧烈搅拌下将剩余物溶于600mL水，过滤析出的沉淀，用水洗,得到的粗品可直接用于下步反应，如用甲醇重结晶，可得无色的化合物(Ⅰ)的结晶硝酸奥昔康唑。
CN201310726742.8A 2013-12-26 2013-12-26 一种硝酸奥昔康唑的制备方法 Pending CN104744372A (zh)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106279038A (zh) * 2016-08-16 2017-01-04 湖南中威制药有限公司 一种硝酸奥昔康唑原料药的合成方法
CN106883180A (zh) * 2017-03-29 2017-06-23 泉州恒卓化工机械科技有限公司 一种硝酸奥昔康唑的快速合成方法

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106279038A (zh) * 2016-08-16 2017-01-04 湖南中威制药有限公司 一种硝酸奥昔康唑原料药的合成方法
CN106883180A (zh) * 2017-03-29 2017-06-23 泉州恒卓化工机械科技有限公司 一种硝酸奥昔康唑的快速合成方法

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Application publication date: 20150701