公开(公告)号：US6008407A

公开(公告)日：1999-12-28

申请号：US185171

申请日：1998-11-03

申请人： Oleg Matveyevich Nefedov ,  Nikolay Vasiljcvich Volchkov ,  Mariya Borisovna Lipkind ,  Ho Seong Lee ,  Young Jun Park ,  Min Hwan Kim

发明人： Oleg Matveyevich Nefedov ,  Nikolay Vasiljcvich Volchkov ,  Mariya Borisovna Lipkind ,  Ho Seong Lee ,  Young Jun Park ,  Min Hwan Kim

IPC分类号： C07C17/25 ,  C07C17/30 ,  C07C25/13 ,  C07C51/58 ,  C07C51/16

CPC分类号： C07C17/30 ,  C07C17/25 ,  C07C25/13 ,  C07C51/093 ,  C07C51/58

摘要： The present invention provides a method of preparing ortho-difluorobenzene derivatives, which comprises (a) providing a mixture of cyclohexenes by reacting chlorotrifluoroethylene (CTFE) and 1.3-diene in a flow reactor and distilling the resultant, and (b) dehydrohalogenating the mixture of cyclohexenes with a phase transition catalyst in :he presence of alkali metal hydroxide at temperature range of 40 to 150.degree. C. without using any organic solvent. The distillate having low boiling point, which is obtained during distillation of the resultant, is recycled into the flow reactor. The present invention also provides a method of preparing 2-chloro-4,5-difluorobenzoic acid, which comprises (a) providing a mixture of 4-chloro-1-methyl-4,5,5-trifluorocyclohexene and 5-chloro-1-methyl-4,4,5-trifluorocyclohexene by reacting chlorotrifluoroethylene (CTFE) and isoprene and distilling the resultant. (b) dehydrohalogenating said mixture in the presence of alkali metal hydroxide and a phase transition catalyst to form 3,4-difluorotoluene, to reacting said 3,4-difluorotoluene with chlorine gas without using any organic solvent to form 2-chloro-4,5-difluorotoluene, (d) photo-reacting said 2-chloro-4,5-difluorotoluene with chlorine gas under a lighting mercury lamp without using any organic solvent to form 2-chloro-4,5-difluorobenzotrichloride, and (e) reacting said 2-chloro-4,5-difluorobenzotrichloride with aqueous acid solution without using any organic solvent. The present invention also provides a method of preparing 2-chloro-4,5-difluorobenzoyl chloride by reacting the 2-chloro-4,5-difluorobenzotrichloride of step (e) above with zinc oxide.

摘要翻译： 本发明提供了一种制备邻二氟苯衍生物的方法，其包括（a）通过在流动反应器中使氯三氟乙烯（CTFE）和1,3-二烯反应提供环己烯的混合物并蒸馏所得物，和（b）脱卤化氢 具有相变催化剂的环己烯：在不使用任何有机溶剂的情况下，在40至150℃的温度范围内存在碱金属氢氧化物。 在蒸馏过程中获得的具有低沸点的馏出物被循环到流动反应器中。 本发明还提供了制备2-氯-4,5-二氟苯甲酸的方法，其包括（a）提供4-氯-1-甲基-4,5,5-三氟环己烯和5-氯-1 - 甲基-4,4,5-三氟环己烯，通过氯三氟乙烯（CTFE）和异戊二烯反应并蒸馏所得物。 （b）在碱金属氢氧化物和相变催化剂的存在下将所述混合物脱卤化氢以形成3,4-二氟甲苯，使所述3,4-二氟甲苯与氯气反应，而不使用任何有机溶剂形成2-氯-4， （d）在照明汞灯下使所述2-氯-4,5-二氟甲苯与氯气进行光反应，而不使用任何有机溶剂形成2-氯-4,5-二氟三氯甲苯，和（e）使 所述2-氯-4,5-二氟三氯甲烷与含水酸溶液不使用任何有机溶剂。 本发明还提供通过使上述步骤（e）的2-氯-4,5-二氟三氯甲苯与氧化锌反应来制备2-氯-4,5-二氟苯甲酰氯的方法。