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Publication number
JP2008143794A5
JP2008143794A5 JP2006329671A JP2006329671A JP2008143794A5 JP 2008143794 A5 JP2008143794 A5 JP 2008143794A5 JP 2006329671 A JP2006329671 A JP 2006329671A JP 2006329671 A JP2006329671 A JP 2006329671A JP 2008143794 A5 JP2008143794 A5 JP 2008143794A5
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Prior art keywords
compound
formula
water
acid
methanol
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JP2006329671A
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Japanese (ja)
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JP2008143794A (en
JP4478140B2 (en
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Publication of JP2008143794A5 publication Critical patent/JP2008143794A5/ja
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Claims (12)

式（１）の化合物またはその塩を、メタノールと水の混合液中で金属塩化反応を行うことにより式（１）の化合物の塩基性塩を得、次いでこれを酸性処理して式（１）の化合物・１／２水和物を得る、式（１）の化合物・１／２水和物の製造方法。
Figure 2008143794
 The compound of formula (1) or a salt thereof is subjected to a metal salinization reaction in a mixed solution of methanol and water to obtain a basic salt of the compound of formula (1), which is then treated with an acid to give a formula (1) A method for producing the compound ½ hydrate of formula (1), wherein the compound ½ hydrate is obtained.
Figure 2008143794
 式（６）の化合物またはその塩を式（７）の化合物と反応させて得られる式（１）の化合物またはその塩を、メタノールと水の混合液中で金属塩化反応を行うことにより式（１）の化合物の塩基性塩を得、次いでこれを酸性処理して式（１）の化合物・１／２水和物を得る、式（１）の化合物・１／２水和物の製造方法。
Figure 2008143794
 The compound of the formula (1) obtained by reacting the compound of the formula (6) or a salt thereof with the compound of the formula (7) or a salt thereof is subjected to a metal salinization reaction in a mixed solution of methanol and water. 1) A basic salt of a compound of the formula (1) is obtained, and then this is treated with an acid to obtain a compound of the formula (1). .
Figure 2008143794
 請求項１または２の方法を含むことを特徴とする、式（１）の化合物の精製方法。
Figure 2008143794
 A process for the purification of a compound of formula (1), characterized in that it comprises a process according to claim 1 or 2.
Figure 2008143794
 金属塩化反応に用いる塩基が、水酸化ナトリウム、水酸化リチウム、炭酸ナトリウム、炭酸カリウム、炭酸リチウム、炭酸水素ナトリウム、炭酸水素カリウム、または炭酸水素リチウムから選択される請求項１〜３のいずれかの方法。   The base used in the metal chlorination reaction is selected from sodium hydroxide, lithium hydroxide, sodium carbonate, potassium carbonate, lithium carbonate, sodium bicarbonate, potassium bicarbonate, or lithium bicarbonate. Method. 金属塩化反応に用いる塩基が、水酸化ナトリウムである請求項１〜３のいずれかの方法。   The method according to any one of claims 1 to 3, wherein the base used for the metal chloride reaction is sodium hydroxide. メタノールと水の混合液が式（１）の化合物１重量部に対して３〜１５容量部である請求項１〜５のいずれかの方法。   The method according to any one of claims 1 to 5, wherein the mixed liquid of methanol and water is 3 to 15 parts by volume with respect to 1 part by weight of the compound of the formula (1). メタノールと水の混合液の混合割合が、メタノール１容量部に対して、水０．０５〜０．４容量部である請求項１〜６のいずれかの方法。   The method according to any one of claims 1 to 6, wherein the mixing ratio of the mixed liquid of methanol and water is 0.05 to 0.4 parts by volume of water with respect to 1 part by volume of methanol. 酸性処理に用いる酸が塩酸である請求項１〜７のいずれかの方法。   The method according to any one of claims 1 to 7, wherein the acid used for the acid treatment is hydrochloric acid. 酸性処理の反応温度が５０℃から９０℃である請求項１〜８のいずれかの方法。   The method according to any one of claims 1 to 8, wherein the reaction temperature of the acid treatment is from 50C to 90C. 式（１）の化合物の塩基性塩を単離せずに水溶液のまま、酸性処理して式（１）の化合物・１／２水和物を得る請求項１〜９のいずれかの方法。   The method according to any one of claims 1 to 9, wherein the basic salt of the compound of the formula (1) is acid-treated in the form of an aqueous solution without isolation to obtain the compound ½ hydrate of the formula (1). 式（１）の化合物の塩基性塩の水溶液を得るために加える塩基の量が、式（１）の化合物の塩基性塩に対して、０．１〜５倍モルであることを特徴とする請求項１〜１０のいずれかの方法。   The amount of the base added to obtain an aqueous solution of the basic salt of the compound of the formula (1) is 0.1 to 5 times mol with respect to the basic salt of the compound of the formula (1). The method according to claim 1. 酸処理工程における溶媒が水であることを特徴とする請求項１〜１１のいずれかの方法。The method according to claim 1, wherein the solvent in the acid treatment step is water.
JP2006329671A 2006-12-06 2006-12-06 Preparation of carbostyril compounds for pharmaceutical use Expired - Fee Related JP4478140B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2006329671A JP4478140B2 (en) 2006-12-06 2006-12-06 Preparation of carbostyril compounds for pharmaceutical use

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP2006329671A JP4478140B2 (en) 2006-12-06 2006-12-06 Preparation of carbostyril compounds for pharmaceutical use

Publications (3)

Publication Number Publication Date
JP2008143794A JP2008143794A (en) 2008-06-26
JP2008143794A5 true JP2008143794A5 (en) 2009-02-12
JP4478140B2 JP4478140B2 (en) 2010-06-09

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Family Applications (1)

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JP2006329671A Expired - Fee Related JP4478140B2 (en) 2006-12-06 2006-12-06 Preparation of carbostyril compounds for pharmaceutical use

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Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104230798B (en) * 2013-06-13 2017-02-15 重庆圣华曦药业股份有限公司 Preparation method of rebamipide
CN104418802B (en) * 2013-09-07 2017-02-22 重庆汇智药物研究院有限公司 rebamipide monohydrate crystal form and preparation method thereof
CN108069901B (en) * 2016-11-16 2020-12-11 重庆圣华曦药业股份有限公司 Novel rebamipide synthesis process
CN111057001A (en) * 2019-12-23 2020-04-24 巨化集团公司制药厂 Preparation method of quinolone malonate compound
CN113248429A (en) * 2021-06-01 2021-08-13 千辉药业（安徽）有限责任公司 Preparation method of rebamipide bulk drug
CN113336700A (en) * 2021-06-15 2021-09-03 大桐制药（中国）有限责任公司 Preparation method of rebamipide

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