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31. 发明授权

US06433168B1 Highly pure phenothiazine compound, production method thereof, production method of intermediate therefor, and hydrate and novel crystal as starting materials for the intermediate 失效
标题翻译：高纯吩噻嗪化合物，其制备方法，其中间体的制备方法，水合物和新型晶体为中间体的起始原料
公开(公告)号：US06433168B1
公开(公告)日：2002-08-13
申请号：US09621782
申请日：2000-07-21
申请人： Shigeya Yamazaki , Hiroyuki Yumoto , Masami Igi
发明人： Shigeya Yamazaki , Hiroyuki Yumoto , Masami Igi
IPC分类号： C07D41700
CPC分类号： C07D453/02
摘要： According to the method of the present invention, an alkali metal compound, dimethyl sulfoxide, trimethyloxosulfonium halide and 3-quinuclidinone are added in a specific order to give the following compound [II]. This compound is, without treatment or isolation, directly reacted with an alkali metal salt of phenothiazine to give the following compound [III], from which the following compound [I] is obtained. During the production of compound [I], a by-produced acidic gas is removed and water is added to ensure industrial, safe and efficient production of compound [I] at a constantly high yield. Inasmuch as the present invention enables production of the following highly pure compound [A] by eliminating hydrogen halide of compound [I] in glyme in the presence of at least one kind of a base selected from potassium hydroxide and potassium alkoxide, compound [A] having a high purity of not less than 85 mol % can be provided.
摘要翻译：根据本发明的方法，以特定的顺序加入碱金属化合物，二甲基亚砜，三甲基锍卤化物和3-奎宁环酮，得到下列化合物[II]。该化合物在不经处理或分离的情况下与吩噻嗪的碱金属盐直接反应，得到以下化合物[III]，由此得到下列化合物[I]。在化合物[I]的生产过程中，除去副产的酸性气体，加入水以确保化合物[I]的工业，安全和有效的生产以不断的高产率。由于本发明能够通过在至少一种选自氢氧化钾和醇钾的碱的存在下，通过除去甘醇二甲醚中的化合物[I]的卤化氢来制备下列高纯度化合物[A]，化合物[A] 可以提供不小于85mol％的高纯度。

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