公开(公告)号：EP1314720A4

公开(公告)日：2004-08-18

申请号：EP01963406

申请日：2001-08-31

申请人： TOKO PHARMACEUTICAL IND CO LTD ,  RES FOUND ITSUU LAB

发明人： KAGECHIKA HIROYUKI ,  NAGANO HIROO

IPC分类号： C07C231/24 ,  C07C233/65 ,  C07C235/84

CPC分类号： C07C233/65 ,  C07C231/24 ,  C07C2602/10 ,  C07C235/84

摘要： A process for producing crystals of 4-[(5,6,7,8-tetra- hydro-5,5,8,8-tetramethyl-2-naphthalenyl)carbamoyl]benzoic acid exhibiting a single endothermic peak near 233°C in differential scanning calorimetry, which comprises the step of recrystallizing crystals of 4-[(5,6,7,8-tetrahydro-5,5,8,8 -tetramethyl-2-naphthalenyl)carbamoyl]benzoic acid from a water-ethanol mixture. This process enables selective production of type II crystals stable to physical impact, and the obtained crystals are free from highly toxic hexane as the residual solvent, thus being suitably usable as an active ingredient in medicines.

公开(公告)号：EP1314720A1

公开(公告)日：2003-05-28

申请号：EP01963406.2

申请日：2001-08-31

申请人： Toko Pharmaceutical Ind. Co. Ltd ,  Research Foundation Itsuu Laboratory

发明人： KAGECHIKA, Hiroyuki ,  NAGANO, Hiroo

IPC分类号： C07C233/65 ,  C07C231/24

CPC分类号： C07C233/65 ,  C07C231/24 ,  C07C2602/10 ,  C07C235/84

摘要： A method for preparing a crystal of 4-[(5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthalenyl)carbamoyl]benzoic acid having a single endothermic peak approximately at 233°C in differential scanning calorimetry, which comprises the step of recrystallizing a crystal of 4-[(5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthalenyl)carbamoyl]benzoic acid from a mixture of water and ethanol. The method enables selective preparation of type-II crystals which are stable against physical impact. The resulting crystals are free from highly toxic hexane as a residual solvent, and preferably used as an active ingredient of pharmaceuticals.

公开(公告)号：EP1314720B1

公开(公告)日：2010-09-29

申请号：EP01963406.2

申请日：2001-08-31

申请人： Toko Pharmaceutical Ind. Co. Ltd ,  Research Foundation Itsuu Laboratory

发明人： KAGECHIKA, Hiroyuki ,  NAGANO, Hiroo

IPC分类号： C07C233/65 ,  C07C231/24

CPC分类号： C07C233/65 ,  C07C231/24 ,  C07C2602/10 ,  C07C235/84

摘要： A process for producing crystals of 4-[(5,6,7,8-tetra- hydro-5,5,8,8-tetramethyl-2-naphthalenyl)carbamoyl]benzoic acid exhibiting a single endothermic peak near 233°C in differential scanning calorimetry, which comprises the step of recrystallizing crystals of 4-[(5,6,7,8-tetrahydro-5,5,8,8 -tetramethyl-2-naphthalenyl)carbamoyl]benzoic acid from a water-ethanol mixture. This process enables selective production of type II crystals stable to physical impact, and the obtained crystals are free from highly toxic hexane as the residual solvent, thus being suitably usable as an active ingredient in medicines.

摘要翻译： 一种制备4-Ä（5,6,7,8-四氢-5,5,8,8-四甲基-2-萘基）氨基甲酰基的重结晶的方法，其具有大约在233℃的单一吸热峰 扫描量热法，其包括从水和乙醇的混合物中重结晶4-Ä（5,6,7,8-四氢-5,5,8,8-四甲基-2-萘基）氨基甲酰基的重氮的步骤 。 该方法能够选择性制备对物理冲击稳定的II型晶体。 所得结晶不含作为残留溶剂的高毒性己烷，优选用作药物的有效成分。