Production of 3,3-dimethyl-2-oxo-butyric acid salt
    1.
    发明授权
    Production of 3,3-dimethyl-2-oxo-butyric acid salt 失效
    制备3,3-二甲基-2-氧代 - 丁酸盐

    公开(公告)号:US4052460A

    公开(公告)日:1977-10-04

    申请号:US650651

    申请日:1976-01-20

    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.

    Process for the preparation of thiophenols
    2.
    发明授权
    Process for the preparation of thiophenols 失效
    制备苯硫酚的方法

    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。