OH, MIN KEUN,오민근,KIM, KI NAM,김기남,SUH, KI HYOUNG,서기형,KWON, DAE GIL,권대길
申请号：
KR1020110037411
公开号：
KR1020120119468A
申请日:
2011.04.21
申请国别(地区):
KR
年份:
2012
代理人:
摘要：
PURPOSE: A partitioning method of racemic 1,4- thiazepine compound is provided to reduce total manufacturing cost by easily purchasing alcohol solvent and organic acid at low cost.CONSTITUTION: A partitioning method of racemic 1,4- thiazepine compound comprises the following steps: dissolving (6R)-6-amino-2-(thiophene-2-yl)-1,4-thiazepan-5-one of chemical formula 1 which is a racemic compound in an alcohol solvent of methanol, ethanol, propanol, and isopropanol performing salt formation by adding organic acid of ascorbic acid, tartaric acid, camphorsulfonic acid cooling the reactant getting and filtering and removing antipode which is educted as crystal vacuum concentrating the filtrate and melting in the chloroform or the methylene chloride and dissolving into KOH or K2CO3 aqueous solution and crystallizing thereof with acetonitrile or ethyl acetate and obtaining (6R)-6-amino-2-(thiophene-2-yl)-1,4-thiazepan-5-one of chemical formula 2. In the first step, the used amount of the alcohol solvent is 6-15 times of the (6R)-6-amino-2-(thiophene-2-yl)-1,4-thiazepan-5-one.COPYRIGHT KIPO 2013본 발명은 라세믹 1,4-티아제핀 화합물의 분할 방법에 관한 것으로서, 좀더 상세하게 설명하면 키랄(Chiral) 특성을 갖는 하기 화학식 1로 표시되는 (6R)-6-아미노-2-(티오펜-2-일)-1,4-티아제판-5-온의 라세미 화합물을 화학적으로 광학 분할(optical resolution)하여 혈압강하제 테모카프릴(Temocapril)의 제조 중간체로 유용한 (S)-에난티오머(enantiomer)인 하기 화학식 2의 (2S,6R)-6-아미노-2-(티오펜-2-일)-1,4-티아제판-5-온을 수득하는 새로운 분할 방법에 관한 것이다.[화학식 1][화학식 2]
