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1. 发明专利

JP2013209432A Method for producing optically active, racemic menthol 有权
标题翻译：用于生产光学活性的，法定的MENTHOL的方法
公开(公告)号：JP2013209432A
公开(公告)日：2013-10-10
申请号：JP2013140738
申请日：2013-07-04
申请人： Basf Se , ビーエーエスエフソシエタス・ヨーロピアBasf Se
发明人： HEYDRICH GUNNAR , GRALLA GABRIELE , RAULS MATTHIAS DR , SCHMIDT-LEITHOFF JOACHIM , EBEL KLAUS DR , KRAUSE WOLFGANG DR , OEHLENSCHLAEGER STEFFEN , JAEKEL CHRISTOPH , FRIEDRICH MARKO , BERGNER EIKE JOHANNES , KASHANI-SHIRAZI NAWID , PACIELLO ROCCO
IPC分类号： C07C29/156 , B01J31/28 , C07B53/00 , C07B61/00 , C07C35/12
CPC分类号： C07C29/56 , C07B2200/07 , C07C29/172 , C07C29/78 , C07C45/62 , C07C45/82 , C07C2601/14 , C07C2601/16 , C07C47/21 , C07C35/12 , C07C35/17
摘要： PROBLEM TO BE SOLVED: To provide a method enabling to manufacture optically active menthol, desirably L-menthol and racemic menthol in a variety of quantity according to the demand without changing an enantioselective catalyst system and/or without excessively obtaining one of products for need of changing a reaction condition.SOLUTION: A method for producing menthol includes a process (a. 1) of obtaining a citronellal by catalyst-hydrogenation of a neral and/or a geranial, a process (b. 1) of obtaining an isopulegol by cyclizing citronellal in the presence of an acid catalyst, a process (c. 1) of purifying the isopulegol by crystallization, and a process (d. 1) of producing menthol by catalyst-hydrogenation of the isopulegol.
摘要翻译：要解决的问题：提供一种能够根据需要以不需要改变对映体选择性催化剂体系，和/或不过度地获得需要的物质的产品之一来制备光学活性薄荷醇，理想的L-薄荷醇和外消旋薄荷醇，改变反应条件。解决方案：制备薄荷醇的方法包括通过催化剂氢化和/或香草醛获得香茅醛的方法（a.1），通过环化获得异焦耳的方法（b.1）在酸催化剂存在下的香茅醛，通过结晶纯化异焦耳的方法（c.1），以及通过异双胍的催化氢化制备薄荷醇的方法（d.1）。

2. 发明专利

JP2013155183A Preparation method of menthol 审中-公开
标题翻译： MENTHOL的制备方法
公开(公告)号：JP2013155183A
公开(公告)日：2013-08-15
申请号：JP2013078582
申请日：2013-04-04
申请人： Basf Se , ビーエーエスエフソシエタス・ヨーロピアBasf Se
发明人： BERGNER EIKE JOHANNES , EBEL KLAUS , THORSTEN JOHANN , OLIVER LOEBER
IPC分类号： C07C29/17 , A23L27/20 , B01J27/232 , B01J31/24 , C07B53/00 , C07B61/00 , C07C29/56 , C07C29/76 , C07C33/025 , C07C35/12 , C07C35/17 , C07C45/29 , C07C47/21
CPC分类号： C07C29/17 , C07B2200/07 , C07C29/172 , C07C45/002 , C07C2601/14 , C12C11/02 , C07C33/025 , C07C35/12 , C07C29/56 , C07C35/17 , C07C47/21
摘要： PROBLEM TO BE SOLVED: To provide a method of asymmetrically synthesizing optical activity menthol from one or more inexpensive achiral starting materials that do not require isolation from a natural supply source.SOLUTION: (a) Optical activity citronellol is obtained by enantio-selectively hydrogenating geraniol, nerol, or a mixture of geraniol and nerol, (b) optical activity citronellal is obtained by reaction of the obtained optical activity citronellol, (c) a mixture containing optical activity isopulegol is obtained by cyclizing the obtained optical activity citronellal, and (d) optical activity menthol is obtained by extracting the optical activity isopulegol from the obtained mixture and then hydrogenating it, or by hydrogenating the optical activity isopulegol contained in the mixture to produce optical activity menthol and then extracting the obtained optical activity menthol from the mixture obtained as a hydrogenated product. Thus, in this method, optical activity menthol is manufactured from geraniol, nerol, or a mixture of geraniol and nerol.
摘要翻译：要解决的问题：提供从不需要与天然供应源分离的一种或多种廉价的非手性起始原料不对称地合成光学活性薄荷醇的方法。解决方案：（a）通过对映选择性氢化香叶醇获得光学活性香茅醇，橙花醇或香叶醇和橙花醇的混合物，（b）通过所得光学活性香茅醇反应获得光学活性香茅醛，（c）通过使获得的光学活性香茅醛环化获得含有光学活性的混合物，）光学活性薄荷醇通过从获得的混合物中提取光学活性异双胍，然后将其氢化，或通过氢化混合物中所含的光学活性异双胍获得光学活性薄荷醇，然后从获得的混合物中提取所得的光学活性薄荷醇氢化产物。因此，在该方法中，光学活性薄荷脑由香叶醇，橙花醇或香叶醇和橙花醇的混合物制成。

3. 发明专利

JP2014159402A Process for preparation of menthol by hydrogenation of isopulegol 审中-公开
标题翻译：通过加氢异烟肼制备精胺的方法
公开(公告)号：JP2014159402A
公开(公告)日：2014-09-04
申请号：JP2013253827
申请日：2013-12-09
申请人： Basf Se , ビーエーエスエフソシエタス・ヨーロピアBasf Se
发明人： GABRIELE GRALLA , GUNNAR HEYDRICH , BERGNER EIKE JOHANNES , KLAUS EBEL
IPC分类号： C07C29/17 , B01J23/88 , B01J37/03 , C07B61/00 , C07C35/12
CPC分类号： C07C29/172 , C07B2200/07 , C07C2601/14 , C07C35/12
摘要： PROBLEM TO BE SOLVED: To provide a process which allows the preparation of substantially diastereoisomerically pure menthol by the hydrogenation of diastereoisomerically pure isopulegol.SOLUTION: The process for preparing racemic or optically active menthol comprises catalytically hydrogenating racemic or optically active isopulegol in the presence of hydrogen, and a catalyst which comprises nickel-, copper-, zirconium- and molybdenum-containing compounds. Concretely, the process prepares L-menthol by continuously catalytically hydrogenating L-isopulegol. In a synthetic method of menthol by the hydrogenation of isopulegol, hydrogenation is carried out under conditions that the hydrogen pressure is 5-200 bar and the temperature is 50-130°C, in the presence of a catalyst containing 30 to 70% by weight of oxygen compounds of nickel, calculated as NiO, 15 to 45% by weight of oxygen compounds of zirconium, calculated as ZrO, 5 to 30% by weight of oxygen compounds of copper, calculated as CuO, and 0.1 to 10% by weight of oxygen compounds of molybdenum, calculated as MoO.
摘要翻译：要解决的问题：提供一种允许通过非对映异构体纯的异双胍的氢化制备基本上非对映异构纯的薄荷醇的方法。溶液：制备外消旋或光学活性薄荷醇的方法包括在氢气存在下催化氢化外消旋或光学活性的异胡，以及包含含镍，铜，锆和钼的化合物的催化剂。具体来说，该方法通过连续催化氢化L-异头process醇来制备L-薄荷醇。在异丙醇氢化的薄荷醇的合成方法中，在氢压为5〜200巴，温度为50〜130℃的条件下，在含有30〜70重量％按NiO计算的镍的氧化合物，以ZrO计算的15〜45重量％的锆的氧化合物，按CuO计的5〜30重量％的铜的氧化合物和0.1〜10重量％钼的氧化合物，以MoO计算。

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