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2. 发明授权

KR100395204B1 특정 결정 형태의 질파테롤 히드로클로라이드, 그의제조방법및이에사용되는중간생성물 失效
标题翻译： 특정결정형태의질파테롤히드로클로라이드，그의제조방법법이용되용되는간간생성물
公开(公告)号：KR100395204B1
公开(公告)日：2003-11-17
申请号：KR1019960020901
申请日：1996-06-12
申请人： 훽스트 뤼쎌 베트 소시에떼아노님
发明人： 이브쉐브레몽 , 장-이브고다르
IPC分类号： C07D487/06
CPC分类号： C07D471/06 , A23K20/137 , Y10S426/807
摘要： Anhydrous crystalline zilpaterol hydrochloride (I), contg. less than 5% of crystals smaller than 15 mu , the rest of the crystals being smaller than 250 mu , is new. Also claimed are (I)-monohydrate and (I)-trihydrate. The claimed prepn. of (I) comprises: (i) forming a super-satd. soln. of (I) in water or in an ethanol/water mixt. at below 50 degrees C; (ii) cooling the soln. to crystallise the monohydrate; (iii) lowering the temp. to below 20 degrees C to crystallise the trihydrate; and (iv) drying to give the desired prod. A variation on the above procedure comprises dissolving (I) in water at below 30 degrees C to give a satd. aq. soln. from which the trihydrate recrystallises spontaneously. Alternatively, a soln. of (I) in a min. amt. of warm water (60-100 degrees C) is poured into a satd. soln. of (I) in a water/alcohol mixt. which has been previously stirred at below 20 degrees C and seeded with trihydrate, to give the trihydrate, which is then dried (all claimed).
摘要翻译：无水结晶齐帕特罗盐酸盐（I）少于5％的晶体小于15亩，其余的晶体小于250亩，是新的。还要求保护（I） - 一水合物和（I） - 三水合物。声称的准备。（I）包括：（i）形成超级饱和脂肪酸。 SOLN。（I）的水溶液或乙醇/水混合物中。在50摄氏度以下; （ii）冷却溶液。使一水合物结晶; （三）降低温度。降至20℃以下以结晶三水合物; 和（iv）干燥以得到期望的产物。上述步骤的变化包括将（I）溶解于低于30℃的水中以得到饱和溶液。水性。 SOLN。三水合物从中自发再结晶。或者，一个soln。（I）in a min。 AMT。温水（60-100摄氏度）倒入一个卫生间。 SOLN。（I）在水/醇混合物中。其先前在低于20℃下搅拌并接种三水合物，以得到三水合物，然后将其干燥（全部要求保护）。

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