公开(公告)号：US4564704A

公开(公告)日：1986-01-14

申请号：US227552

申请日：1981-01-22

申请人： Karlfried Dickore ,  Hans D. Engels ,  Hans Kratzer ,  Walter Merz

发明人： Karlfried Dickore ,  Hans D. Engels ,  Hans Kratzer ,  Walter Merz

IPC分类号： C07C45/63 ,  C07C51/00 ,  C07C59/185 ,  C07C51/285 ,  C07C51/373

CPC分类号： C07C59/185 ,  C07C45/63 ,  C07C51/00

摘要： Dichloropinacolone is produced by introducing into pinacolone twice the molar amount of chlorine, the exothermic reaction mass being cooled initially to maintain the temperature below about 50.degree. C. until about 60 to 80% of the chlorine has been introduced, and then heating the reaction mass to a temperature above 50.degree. C. during introducing of the remainder of the chlorine, thereby to produce dichloropinacolone, and terminating chlorine introduction when the dichloropinacolone content of the reaction mass is at least about 97%. The molten product is added to an aqueous solution of an alkali maintained at a temperature of at least about 50.degree. C., the alkali being present in more than three times the molar amount of the dichloropinacolone. To the resulting solution of a salt of 3,3-dimethyl-2-hydroxy-butyric acid, brought to a pH of about 9 to 12, there is added approximately the stoichiometric amount of potassium permanganate. Solid MnO.sub.2 precipitates out and is separated from the substantially pure dissolved salt of 3,3-dimethyl-2-oxo-butyric acid. The product is a known compound suited for further syntheses.

摘要翻译： 通过将频倍他康酮引入两倍于氯的摩尔量来产生二氯可乐乐，最初冷却放热反应物质以保持温度低于约50℃，直到引入约60至80％的氯，然后加热反应物质 在导入剩余的氯的过程中温度高于50℃，从而产生二氯靛那烯，并且当反应物质的二氯新戊酮酮含量为至少约97％时终止氯引入。 将熔融产物加入到保持在至少约50℃温度的碱的水溶液中，碱的存在量是氯苯腈的摩尔量的三倍以上。 向所得到的3,3-二甲基-2-羟基 - 丁酸的盐溶液中加入大约9-12的pH，加入大约化学计量的高锰酸钾。 固体MnO 2析出并与3,3-二甲基-2-氧代 - 丁酸的基本上纯的溶解盐分离。 该产物是适用于进一步合成的已知化合物。

公开(公告)号：US4898974A

公开(公告)日：1990-02-06

申请号：US726218

申请日：1985-04-23

申请人： Karlfried Dickore ,  Hans D. Engels ,  Hans Kratzer ,  Walter Merz

发明人： Karlfried Dickore ,  Hans D. Engels ,  Hans Kratzer ,  Walter Merz

IPC分类号： C07C45/63 ,  C07C51/00 ,  C07C59/185

CPC分类号： C07C59/185 ,  C07C45/63 ,  C07C51/00

摘要： Dichloropinacolone is produced by introducing into pinacolone twice the molar amount of chlorine, the exothermic reaction mass being cooled initially to maintain the temperature below about 50.degree. C. until about 60 to 80% of the chlorine has been introduced, and then heating the reaction mass to a temperature above 50.degree. C. during introducing of the remainder of the chlorine, thereby to produce dichloropinacolone, and terminating chlorine introduction when the dichloropinacolone content of the reaction mass is at least about 97%. The molten product is added to an aqueous solution of an alkali maintained at a temperature of at least about 50.degree. C., the alkali being present in more than three times the molar amount of the dichloropinacolone. To the resulting solution of a salt of 3,3-dimethyl-2-hydroxy-butyric acid, brought to a pH of about 9 to 12, there is added approximately the stoichiometric amount of potassium permanganate. Solid MnO.sub.2 precipitates out and is separated from the substantially pure dissolved salt of 3,3-dimethyl-2-oxo-butyric acid. The produce is a known compound suited for further syntheses.

摘要翻译： 通过将频倍他康酮引入两倍于氯的摩尔量来产生二氯可乐乐，最初冷却放热反应物质以保持温度低于约50℃，直到引入约60至80％的氯，然后加热反应物质 在导入剩余的氯的过程中温度高于50℃，从而产生二氯一可乐酮，并且当反应物质的二氯新戊酮酮含量为至少约97％时终止氯引入。 将熔融产物加入到保持在至少约50℃温度的碱的水溶液中，碱的存在量是氯苯腈的摩尔量的三倍以上。 向所得到的3,3-二甲基-2-羟基 - 丁酸的盐溶液中加入大约9-12的pH，加入大约化学计量的高锰酸钾。 固体MnO 2析出并与3,3-二甲基-2-氧代 - 丁酸的基本上纯的溶解盐分离。 该产物是适用于进一步合成的已知化合物。