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公开(公告)号:US3767647A
公开(公告)日:1973-10-23
申请号:US3767647D
申请日:1971-01-11
Applicant: TOA GOSEI CHEM IND
Inventor: HIROSE T , MATSUBARA T
IPC: C07D201/04 , C07D41/00
CPC classification number: C07D201/04
Abstract: A HIGH PURITY W-LAUROLACTAM IS PREPARED FROM A CRUDE CYCLODODECANONE OXIME CONTAINING 5% BY WEIGHT OR LESS OF CYCLODODECANONE BY SUBJECTING THE OXIME TO THE BECKMANN REARRANGEMENT REACTION IN THE PRESENCE OF SULFURIC ACID HAVING A CONCENTRATION OF 98% BY WEIGHT OR MORE OR FUMING SULFURIC ACID CONTAINING 20% BY WEIGHT OR LESS OF SULFURIC-ANHYDRIDE, SEPARATING THE THUS FORMED W-LAUROLACTAM FROM THE REACTION MIXTURE, DISSOLVING THE RESULTING W-LAUROLACTAM N A LIQUID AROMATIC HYDROCARBON, WASHING THE SOLUTION WITH AN ALKALI SOLUTION AT A TEMPERATURE OF 60* TO 120* C., AND RECOVERING W-LAUROLACTAM.
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公开(公告)号:US3808275A
公开(公告)日:1974-04-30
申请号:US12735071
申请日:1971-03-23
Applicant: TOA GOSEI CHEM IND
Inventor: HIROSE T , MATSUBARA T
IPC: C07C131/00
Abstract: A HIGH-PURITY KETOXIME CAN BE OBTAINED IN A HIGH YIELD (HIGH CONVERSION AND HIGH SELECTIVITY) BY REACTING AT LEAST ONE KETONE WITH HYDROXYLAMINE OR A SALT THEREOF IN THE PRESENCE OF A TIN-CONTAINING COMPOUND, EVEN WHEN THE PH OF THE REACTION SYSTEM IS 6 OR HIGHER.
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公开(公告)号:US3714244A
公开(公告)日:1973-01-30
申请号:US3714244D
申请日:1971-04-06
Applicant: TOA GOSEI CHEM IND
Inventor: OKADA Y , MATSUBARA T
Abstract: Crude 1,12-dodecanedioic acid obtained by oxidation of cyclododecanol and/or cyclododecanone by nitric acid is purified by dissolving the crude 1,12-dodecanedioic acid in an aqueous nitric acid solution containing 40 to 80 percent by weight of nitric acid at 85*-105*C, passing the resulting solution through a filter aid diatomaceous earth having particle sizes of 1-100 microns, cooling the resulting filtrate to 40*-90*C thereby to crystallize 1,12-dodecanedioic acid. The thus purified 1,12dodecanedioic acid has a good purity and a less susceptibility of discoloration appearing when dissolved in an alkali.
Abstract translation: 通过用硝酸将环十二烷醇和/或环十二烷酮氧化得到的粗制1,12-十二烷二酸通过将粗制的1,12-十二烷二酸溶解在含有40-80%(重量)硝酸的硝酸水溶液的85℃水溶液中进行纯化 -105℃,使得到的溶液通过一个具有1-100微米粒度的助滤剂硅藻土,将所得滤液冷却至40-90℃,从而使1,12-十二烷二酸结晶。 如此纯化的1,12-十二烷二酸具有良好的纯度,并且当溶解在碱中时出现较少的变色的易感性。
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