Process for the manufacture of thiophosphoryl chloride
    4.
    发明授权
    Process for the manufacture of thiophosphoryl chloride 失效
    制备硫代磷酰氯的方法

    公开(公告)号:US06251350B1

    公开(公告)日:2001-06-26

    申请号:US09337088

    申请日:1999-06-21

    IPC分类号: C01B2510

    CPC分类号: C01B25/10

    摘要: The present invention relates to an improved process for the preparation of thiophosphoryl chloride which is useful as an intermediate for the synthesis of insecticidally active compounds. The improvement comprises the presence in the reaction mixture of a catalytic amount of a nitroxide free radical of the following general formula: wherein R1, R2, R3 and R4 represent an alkyl group.

    摘要翻译: 本发明涉及一种制备硫代磷酰氯的改进方法,其可用作合成杀虫活性化合物的中间体。 改进包括在反应混合物中存在催化量的以下通式的氮氧自由基:其中R1,R2,R3和R4表示烷基。

    Process for making 2-(methylthio)-5-(trifluoromethyl)-1,3,4-thiadiazole
using methyldithiocarbazinate with trifluoroacetic acid with selective
removal of 2,5-bis(methylthio)-1,3,4-thiadiazole
    5.
    发明授权
    Process for making 2-(methylthio)-5-(trifluoromethyl)-1,3,4-thiadiazole using methyldithiocarbazinate with trifluoroacetic acid with selective removal of 2,5-bis(methylthio)-1,3,4-thiadiazole 有权
    使用甲基二硫代肼基甲酸酯与三氟乙酸制备2-(甲硫基)-5-(三氟甲基)-1,3,4-噻二唑的方法,选择性除去2,5-二(甲硫基)-1,3,4-噻二唑

    公开(公告)号:US6034245A

    公开(公告)日:2000-03-07

    申请号:US215492

    申请日:1998-12-18

    IPC分类号: C07D285/12 C07D285/125

    CPC分类号: C07D285/125 Y02P20/582

    摘要: The present invention provides a process for making 2-(methylthio)-5-(trifluoromethyl)-1,3,4-thiadiazole. The process includes the steps of reacting methyidithiocarbazinate with trifluoroacetic acid, in the absence of phosphorus trichloride, to form a mixture of 2-(methylthio)-5-(trifluoromethyl)-1,3,4-thiadiazole and 2,5-bis-(methylthio)-1,3,4-thiadiazole. Further, the process of the present invention includes selectively removing the 2,5-bis-(methylthio)-1,3,4-thiadiazole by acidifying the reaction mixture, and then separating the aqueous and organic phases.

    摘要翻译: 本发明提供制备2-(甲硫基)-5-(三氟甲基)-1,3,4-噻二唑的方法。 该方法包括在不存在三氯化磷的情况下使甲基二硫代肼基甲酸酯与三氟乙酸反应,形成2-(甲硫基)-5-(三氟甲基)-1,3,4-噻二唑和2,5-双 (甲硫基)-1,3,4-噻二唑。 此外,本发明的方法包括通过酸化反应混合物,然后分离水相和有机相,选择性地除去2,5-双(甲硫基)-1,3,4-噻二唑。

    Process for producing stable, low odor S,S,S-tributylphosphorothrithiote
    8.
    发明授权
    Process for producing stable, low odor S,S,S-tributylphosphorothrithiote 失效
    生产稳定,低气味的S,S,S-三丁基磷酸二硫代磷酸酯的方法

    公开(公告)号:US5831112A

    公开(公告)日:1998-11-03

    申请号:US878857

    申请日:1997-06-20

    IPC分类号: C07F9/17

    CPC分类号: C07F9/17

    摘要: The invention is directed to a process for producing a stable, low odor S,S,S-tributylphosphorotrithioate having a level of dibutyl disulfide of 0.3% by weight or less. The process broadly includes the steps of a) reacting S,S,S-tributylphosphorotrithioite with an oxidizing agent to produce a crude S,S,S-tributylphosphorotrithioate, b) treating the crude product with sodium bisulfite to decompose any excess oxidizing agent, c) adding a caustic solution having a caustic concentration of from 25 to 50% by weight directly to the reaction mixture of step b), the addition of said caustic solution being stopped once the total caustic concentration is less than 10% by weight and once the pH is constant, and d) phase separating S,S,S-tributylphosphorotrithioate from the mixture of step c).

    摘要翻译: 本发明涉及一种生产具有0.3重量%以下的二丁基二硫化物水平的稳定,低气味的S,S,S-三丁基次磷酸二硫代磷酸酯的方法。 该方法广泛地包括以下步骤:a)使S,S,S-三丁基磷酸三铁铵与氧化剂反应以产生粗S,S,S-三丁基磷酸二硫代酸酯,b)用亚硫酸氢钠处理粗产物以分解任何过量的氧化剂,c )将苛性碱浓度为25〜50重量%的苛性碱溶液直接加入到步骤b)的反应混合物中,一旦苛性碱总浓度低于10重量%,就停止加入所述苛性碱溶液 pH恒定,d)从步骤c)的混合物中分离S,S,S-三丁基次磷酸二硫代磷酸酯。

    Process for the production of oxiranes
    10.
    发明授权
    Process for the production of oxiranes 失效
    生产环氧乙烷的方法

    公开(公告)号:US5256802A

    公开(公告)日:1993-10-26

    申请号:US504784

    申请日:1990-04-03

    CPC分类号: C07D303/08 C07D301/02

    摘要: Oxiranes are made from ketones by heating a ketone which is preferably an alkyl ketone to a temperature of from about 60.degree. to about 90.degree. C. (preferably about 80.degree. C.) in the presence of a sulfonium salt, a quaternary ammonium salt and a potassium hydroxide solution which is at least 61% potassium hydroxide. It is preferred that no organic solvent be included in the reaction mixture. The potassium hydroxide is generally included in an amount such that for every mole of ketone, from about 3 to about 4 moles of potassium hydroxide are present. The sulfonium salt is generally used in an amount of at least 1.1 moles for each mole of ketone. The quaternary ammonium salt is generally used in an amount of from about 1 to about 5 mol % based on moles of ketone present.

    摘要翻译: 通过在锍盐,季铵盐和季铵盐存在下将优选烷基酮的酮加热至约60℃至约90℃(优选约80℃)的温度,由环酮衍生得到环烷烃, 至少61%氢氧化钾的氢氧化钾溶液。 优选在反应混合物中不含有机溶剂。 氢氧化钾通常含有的量使得对于每摩尔酮,存在约3至约4摩尔的氢氧化钾。 锍盐的用量通常为每摩尔酮至少1.1摩尔。 季铵盐的使用量通常以所存在的酮的摩尔数计约1至约5mol%。