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    • 4. 发明授权
    • Process for the preparation of tetrachloro-1,4-benzoquinone
    • 制备四氯-1,4-苯醌的方法
    • US5559257A
    • 1996-09-24
    • US392469
    • 1995-02-22
    • Otto ArndtWolfgang Tronich
    • Otto ArndtWolfgang Tronich
    • B01J27/128C07B61/00C07C46/00C07C46/06C07C50/24C07C50/20
    • C07C46/06
    • The invention relates to a process for the preparation of tetrachloro-1,4-benzoquinone of high purity by the action of chlorine and concentrated hydrochloric acid on hydroquinone, which involves introducing a portion of the hydroquinone to be employed into initially introduced hydrochloric acid containing catalytic amounts of iron(III) ions and an anionic dispersant, introducing chlorine gas into this solution at a temperature from 20.degree. to 107.degree. C., then adding the residual quantity of hydroquinone as a solid or in solution, raising the temperature to from 80.degree. to 107.degree. C. while continuing to pass in gaseous chlorine, adding, after the introduction of gaseous chlorine has ended, a relatively high-boiling organic solvent which is not miscible with hydrochloric acid, and subsequently subjecting the reaction mixture to thermal aftertreatment.
    • 本发明涉及通过氯和浓盐酸对氢醌的作用制备高纯度的四氯-1,4-苯醌的方法,其包括将待使用的一部分氢醌引入含有催化剂的初始引入的盐酸中 量的铁(III)离子和阴离子分散剂,在20至107℃的温度下将氯气引入该溶液中,然后加入残留量的氢醌作为固体或溶液,将温度升至80 在继续通入气态氯的同时,在气态氯引入结束后,加入与盐酸不混溶的相对高沸点的有机溶剂,随后使反应混合物进行热后处理。
    • 10. 发明授权
    • Process for the manufacture of 3-amino-1-phenylpyrazol-5-one
    • 3-氨基-1-苯基吡唑-5-酮的制备方法
    • US4410707A
    • 1983-10-18
    • US285469
    • 1981-07-21
    • Wolfgang TronichWolfgang RieperPeter Bohme
    • Wolfgang TronichWolfgang RieperPeter Bohme
    • C07D231/22C07D231/38C07D231/52
    • C07D231/52
    • The preparation of 3-amino-1-phenylpyrazol-5-one by heating phenylhydrazine and a lower cyanoacetic acid alkyl ester in a polar solvent, using a lower alcoholate of an alkali metal as the condensation agent, leads to particularly high yields and quality, if the phenylhydrazine and 1 to 1.2 moles of the alcoholate are initially taken, the cyanoacetic ester is metered in and the reaction is carried out at 105.degree. to 140.degree. C., volatile alcohols which have been liberated from the ester and, if appropriate, from the alcoholate being distilled off at the reaction temperature. It is advantageous to employ the phenylhydrazine in an excess of up to about 200 mole % and to select, as the polar solvent, an alcohol or ether having a boiling point above 105.degree. C.
    • 使用碱金属的低级醇化物作为缩合剂,通过在极性溶剂中加热苯肼和低级氰基乙酸烷基酯来制备3-氨基-1-苯基吡唑-5-酮导致特别高的产率和质量, 如果最初采用苯肼和1至1.2摩尔醇化物,则将氰乙酸酯计量并在105至140℃进行反应,从酯中释放的挥发性醇,如果合适的话, 从醇化物在反应温度下蒸馏掉。 使用过量高达约200摩尔%的苯肼是有利的,并且选择沸点高于105℃的醇或醚作为极性溶剂。