公开(公告)号：US3825532A

公开(公告)日：1974-07-23

申请号：US19232771

申请日：1971-10-26

Applicant: AQUITAINE TOTAL ORGANICO

Inventor： KERN R ,  POULAIN C ,  TOCK F

IPC: C07D201/04 ,  C07D41/00

CPC classification number: C07D201/04

Abstract: A PROCESS FOR REARRANGING CYCLODODECANONEOXIME INTO PURE CYCLODODECALACTAME, CHARACTERIZED BY THE FACT THAT THE OXIME, CONVERTED INTO OXIME CHLORHYDRATE, IS MADE INTO A SOLUTION WITH A SELECTIVE SOLVENT, IN THE PRESENCE OF A SMALL QUANTITY OF CATALYST, CHOSEN FROM THE GROUP OF ACID HALIDES AND OXYHALIDES, AND THEN HEATED TO A TEMPERATURE OF BETWEEN 65 AND 110* C. FOR ONE TO TWO HOURS, THE RESULTING HYDROCHLORIC ACID IS DRAWN OFF BY MEANS OF A FLOW OF GAS WHILE MAINTAINING THE REFLUX TEMPERATURE OF THE SOLVENT, THE REACTION MIXTURE IS WASHED WHILE HOT WITH AN ALKALINE AQUEOUS SOLUTION, THE ORGANIC PHASE CONTAINING THE LACTAME IS WASHED IN HOT WATER UNTIL BECOMES NEUTRAL, AND THE LACTAME IS RECOVERED BY CRYSTALLIZATION OR DISTILLATION OF THE SOLVENT. THE QUANTITY OF CATALYST USED RANGES FROM 0.5 TO 5%, AND PREFERABLY 1 TO 2%, OF THE WEIGHT OF OXIME. THE SOLVENT IS PREFERABLY SELECTED FROM ALKANES, CYCLOALKANES, SUBSTITUTED ALKANE AND CYCLOALKANE DERIVATIVES, AND HALOGENATED ALKANE AND CYCLOALKANE DERIVATIVES.