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公开(公告)号：US4006186A
公开(公告)日：1977-02-01
申请号：US466312
申请日：1974-05-02
IPC分类号： C07C149/00 , C07C149/12
CPC分类号： C07C323/00
摘要： Process for the production of thiophenols of the formula ##STR1## in which N IS AN INTEGER FROM 0 TO 5, INCLUSIVE, ANDR is hydroxy, nitro, halogen, alkyl of from 1 to 6 carbon atoms, alkoxy of from 1 to 6 carbon atoms, amino, monoalkylamino or dialkylamino.Which process comprises reacting, in a first step, the corresponding phenylsulfonic acid chloride with hydrazine, hydriodic acid and hydrochloric acid to give the corresponding sulfonehydrazide; and reacting the product so formed, in the second step, to give the corresponding disulfide; and then splitting the resulting material, in the third step, with hydrazine and alkali to form a thiophenolate from which the thiophenol can be liberated by treatment with a mineral acid.
摘要翻译： 制备其中N为0至5，包含和R 1的整数的式（I）的苯硫酚的方法是羟基，硝基，卤素，1至6个碳原子的烷基，1的烷氧基 至6个碳原子，氨基，单烷基氨基或二烷基氨基。
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公开(公告)号：US4052460A
公开(公告)日：1977-10-04
申请号：US650651
申请日：1976-01-20
IPC分类号： C07C49/16 , C07C45/00 , C07C45/63 , C07C51/00 , C07C51/373 , C07C59/01 , C07C59/185 , C07C67/00
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.
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