公开(公告)号：US20060163159A1

公开(公告)日：2006-07-27

申请号：US10513564

申请日：2003-04-08

申请人： Raymond Jones ,  Alan Whitton ,  Colin Bennie ,  David Ritchie ,  Pascal Bugnon

发明人： Raymond Jones ,  Alan Whitton ,  Colin Bennie ,  David Ritchie ,  Pascal Bugnon

IPC分类号： B01D11/04 ,  A61K31/55

CPC分类号： C07D311/76

摘要： 3-Isochromanone is prepared by partially chlorinating o-tolylacetic acid with sulphuryl chloride or chlorine gas in an inert organic solvent in the presence of a free radical initiator. The 2-chloromethylphenylacetic acid first obtained is converted to 3-isochromanone by treatment with a base and separated from unreacted o-tolylacetic acid, which is in the form of a salt, by a phase separation technique. The separated o-tolylacetic acid salt is converted to o-tolylacetic acid by controlled acidification and the o-tolylacetic acid is extracted for re-use. The invention reduces the formation of unwanted, over-chlorinated by-products and leads to a more efficient process.

公开(公告)号：US07491834B2

公开(公告)日：2009-02-17

申请号：US10513564

申请日：2003-04-08

申请人： Raymond Vincent Heavon Jones ,  Alan John Whitton ,  Colin John Bennie ,  David John Ritchie ,  Pascal Bugnon

发明人： Raymond Vincent Heavon Jones ,  Alan John Whitton ,  Colin John Bennie ,  David John Ritchie ,  Pascal Bugnon

IPC分类号： C07D311/00

CPC分类号： C07D311/76

摘要： 3-Isochromanone is prepared by partially chlorinating o-tolylacetic acid with sulphuryl chloride or chlorine gas in an inert organic solvent in the presence of a free radical initiator. The 2-chloromethylphenylacetic acid first obtained is converted to 3-isochromanone by treatment with a base and separated from unreacted o-tolylacetic acid, which is in the form of a salt, by a phase separation technique. The separated o-tolylacetic acid salt is converted to o-tolylacetic acid by controlled acidification and the o-tolylacetic acid is extracted for re-use. The invention reduces the formation of unwanted, over-chlorinated by-products and leads to a more efficient process.

摘要翻译： 通过在惰性有机溶剂中，在自由基引发剂的存在下，用硫酰氯或氯气部分氯化邻甲苯乙酸来制备3-异色满酮。 首先将得到的2-氯甲基苯乙酸通过用碱处理转化为3-异色满酮，并通过相分离技术从盐形式的未反应的邻甲苯乙酸中分离出来。 通过控制酸化将分离的邻甲苯基乙酸盐转化为邻甲苯乙酸，并将邻甲苯基乙酸萃取再次使用。 本发明减少了不需要的过氯化副产物的形成并导致更有效的方法。