Process for the preparation of vinylphosphonic dichloride
    1.
    发明授权
    Process for the preparation of vinylphosphonic dichloride 失效
    乙烯基膦酸二氯化物的制备方法

    公开(公告)号:US4761252A

    公开(公告)日:1988-08-02

    申请号:US90229

    申请日:1987-08-27

    CPC分类号: C07F9/42

    摘要: The invention relates to a process for the preparation of vinylphosphonic dichloride, in which a 2-chloroethanephosphonate of the formula ##STR1## or a mixture of the two esters, is reacted with thionyl chloride at a temperature of 60.degree. to 160.degree. C. in the presence of a catalyst which contains tertiary phosphines, quaternary ammonium or phosphonium salts or alkali metal or alkaline-earth metal halides.During this reaction, any thionyl chloride which may be present is removed by distillation subsequent to this reaction, the mixture remaining is heated to 140.degree. to 200.degree. C., and the vinylphosphonic dichloride produced during this is removed by distillation.

    摘要翻译: 本发明涉及一种制备乙烯基膦酸二氯化物的方法,其中将式(II)的2-氯乙基膦酸盐或两种酯的混合物与亚硫酰氯在60至160℃的温度下反应。 在含有叔膦,季铵或鏻盐或碱金属或碱土金属卤化物的催化剂的存在下。 在该反应中,在该反应之后,通过蒸馏除去可能存在的任何亚硫酰氯,将剩余的混合物加热至140℃至200℃,并通过蒸馏除去其中产生的乙烯基膦酰氯。

    Process for the preparation of vinylphosphonic dichloride
    2.
    发明授权
    Process for the preparation of vinylphosphonic dichloride 失效
    乙烯基膦酸二氯化物的制备方法

    公开(公告)号:US4761251A

    公开(公告)日:1988-08-02

    申请号:US089964

    申请日:1987-08-27

    IPC分类号: B01J31/00 C07B61/00 C07F9/42

    CPC分类号: C07F9/42

    摘要: The invention relates to a process for the preparation of vinylphosphonic dichloride through elimination of hydrogen chloride from 2-chloroethanephosphonic dichloride in the presence of catalysts. The catalysts used are tertiary phosphines, quaternary ammonium or phosphonium salts or alkali metal or alkaline-earth metal halides. When triphenyl phosphine is used as the catalyst, the reaction is carried out under reduced pressure at a temperature of 130.degree. to 166.degree. C. and the vinylphosphonic dichloride produced is simultaneously removed by distillation under reduced pressure. When the other catalysts are used, the process can be carried out at atmospheric pressure or reduced pressure and at temperatures of about 130.degree. to 220.degree. C. and the vinylphosphonic dichloride produced can be removed by distillation simultaneously with or subsequent to the reaction.

    摘要翻译: 本发明涉及通过在催化剂存在下从2-氯乙烷膦酸二氯中除去氯化氢来制备乙烯基膦酸二氯化物的方法。 所用的催化剂是叔膦,季铵或鏻盐或碱金属或碱土金属卤化物。 当使用三苯基膦作为催化剂时,反应在130〜166℃的温度下进行减压蒸馏,同时通过减压蒸馏同时除去生成的乙烯基膦酸二氯。 当使用其它催化剂时,该方法可以在大气压或低压下和在约130℃至220℃的温度下进行,并且所产生的乙烯基膦酸二氯化物可以在反应或反应后同时通过蒸馏除去。

    Process for the preparation of 2-chloroethanephosphonic dichloride
    3.
    发明授权
    Process for the preparation of 2-chloroethanephosphonic dichloride 失效
    2-氯乙烷膦酸二氯化物的制备方法

    公开(公告)号:US4749524A

    公开(公告)日:1988-06-07

    申请号:US89827

    申请日:1987-08-27

    CPC分类号: C07F9/42

    摘要: The invention relates to a process for the preparation of 2-chloroethanephosphonic dichloride through reaction of a 2-chloroethanephosphonate of the formula ##STR1## or a mixture of the two esters, with thionyl chloride at a temperature of 60.degree. to 160.degree. C. In this reaction, tertiary phosphines, quaternary ammonium or phosphonium salts or alkali metal or alkaline-earth metal halides are employed as catalysts. The thionyl chloride is introduced into the initially introduced ester.

    摘要翻译: 本发明涉及一种制备2-氯乙烷膦酸二氯化物的方法,该方法是将式(Ⅱ)所示的2-氯乙基膦酸酯与式(Ⅱ)的混合物与亚硫酰氯反应,温度为60℃至 160℃。在该反应中,使用叔膦,季铵或鏻盐或碱金属或碱土金属卤化物作为催化剂。 将亚硫酰氯引入初始引入的酯中。

    Radiation-sensitive compounds, radiation-sensitive mixture prepared
therewith and copying material
    6.
    发明授权
    Radiation-sensitive compounds, radiation-sensitive mixture prepared therewith and copying material 失效
    辐射敏感性化合物,其制备的辐射敏感性混合物和复制材料

    公开(公告)号:US5114816A

    公开(公告)日:1992-05-19

    申请号:US431221

    申请日:1989-11-03

    摘要: The invention relates to novel radiation-sensitive compounds which are esters or amides of a 1,2-naphthoquinone-(2)-diazide-4-sulfonic acid of the general formula ##STR1## in which R.sub.1 and R.sub.2 are identical or different and denote hydrogen, an alkyl group, an alkyl ether group or an alkyl thioether group whose carbon chains may be interrupted by ether oxygen atoms, an acylamino group, carboxylic acid ester group, sulfonic acid ester group or sulfonamide group,R.sub.1 and R.sub.2 not being hydrogen at the same time.The compounds are used as radiation-sensitive components in radiation-sensitive mixtures with which corresponding copying materials can be produced. The compounds have an absorption which is directed towards longer wavelengths matching the emission range of commercially available radiation sources. They also make it possible, in a reliable and practical manner, to carry out negativeworking image reversal processes.

    摘要翻译: 本发明涉及新的辐射敏感化合物,它们是通式为(I)的1,2-萘醌 - (2) - 二叠氮-4-磺酸的酯或酰胺,其中R 1和R 2相同或 不同的表示氢,烷基,烷基醚基或其碳链可被醚氧原子间隔的烷基硫醚基,酰氨基,羧酸酯基,磺酸酯基或磺酰胺基,R1和R2不是 同时是氢。 这些化合物用作辐射敏感性混合物中的辐射敏感组分,可以制备相应的复印材料。 这些化合物具有吸收,该吸收指向与市售辐射源的发射范围匹配的较长波长。 它们也使得以可靠和实际的方式实现负面的图像反转过程成为可能。

    Process for the preparation of 2-chloroethanephosphonyl dichloride
    8.
    发明授权
    Process for the preparation of 2-chloroethanephosphonyl dichloride 失效
    2-氯乙酰膦酰氯的制备方法

    公开(公告)号:US4855087A

    公开(公告)日:1989-08-08

    申请号:US127175

    申请日:1987-12-01

    申请人: Herbert Siegel

    发明人: Herbert Siegel

    CPC分类号: C07F9/42

    摘要: The invention relates to a process for the preparation of 2-chloroethanephosphonyl dichloride by reaction of an ester of 2-chloroethanephosphonic acid of the formula ##STR1## or a mixture of the two esters with thionyl chloride at a temperature of 60.degree. to 160.degree. C. Phosphine oxides are employed as catalysts therein. The thionyl chloride is added to the initially introduced ester.

    摘要翻译: 本发明涉及一种制备2-氯乙烷膦酰基二氯化物的方法,该方法是将式(Ⅱ)所示的2-氯乙酰膦酸的酯与式(Ⅱ)的混合物与亚硫酰氯在60℃的温度下反应 DEG至160℃。使用氧化膦作为其中的催化剂。 将亚硫酰氯加入到初始引入的酯中。

    Process for preparing substituted
1,2-naphthoquinone-(2)-diazide-4-sulfonic acid esters and their use in
a radiation-sensitive mixture
    10.
    发明授权
    Process for preparing substituted 1,2-naphthoquinone-(2)-diazide-4-sulfonic acid esters and their use in a radiation-sensitive mixture 失效
    制备取代的1,2-萘醌 - (2) - 二硫代-4-磺酸酯的方法及其在辐射敏感性混合物中的用途

    公开(公告)号:US5082932A

    公开(公告)日:1992-01-21

    申请号:US431182

    申请日:1989-11-03

    摘要: The invention relates to a process for preparing 1,2-naphthoquinone-(2)-diazide-4-sulfonic acid esters of the general formula I ##STR1## which are substituted in at least one of the positions 5, 6, 7 or 8 by R=halogen, alkoxy groups or alkoxycarbonyl groups and in which X denotes an aryl group. The process comprises steps in whicha) suitably substituted .beta.-naphthol is nitrosated,b) sulfonation with alkali hydrogensulfite and acid in position 4 and reduction are carried out,c) the naphthalenesulfonic acid derivative is oxidized,d) the 1,2-naphthoquinone-4-sulfonic acid formed is reacted with toluenesulfonohydrazide in an organic solvent at temperatures from 20.degree. to 100.degree. C.,e) the naphthoquinonediazide compound is converted with chlorosulfonic acid or chlorosulfonic acid/thionyl chloride into the sulfonyl chloride, and f) the sulfonyl chloride is condensed with a phenolic component, a purification of the respective intermediate product by reprecipitation or recrystallization being unnecessary.The process makes a simple technical procedure possible with good yield. The compounds prepared, in particular the 1,2-naphthoquinone-(2)-diazide-4-sulfonic acid esters substituted by 6-alkoxycarbonyl groups or by 7-alkoxy groups, are used as radiation-sensitive components in radiation-sensitive mixtures.

    摘要翻译: 本发明涉及一种制备通式I(I)的1,2-萘醌 - (2) - 二叠氮-4-磺酸酯的方法,它在至少一个位置5,6, 7或8,其中R =卤素,烷氧基或烷氧基羰基,其中X表示芳基。 该方法包括以下步骤:a)适当取代的β-萘酚被亚硝化,b)用碱性亚硫酸氢盐和酸在4位磺化并进行还原,c)萘磺酸衍生物被氧化,d)1,2-萘醌 形成的4-磺酸与甲苯磺酰肼在有机溶剂中在20〜100℃的温度下反应,e)萘醌二叠氮化合物用氯磺酸或氯磺酸/亚硫酰氯转化成磺酰氯,f) 磺酰氯与酚成分缩合,通过再沉淀或重结晶不需要纯化各中间产物。 该过程使得一个简单的技术程序可以获得良好的收益。 制备的化合物,特别是被6-烷氧基羰基或7-烷氧基取代的1,2-萘醌 - (2) - 二叠氮-4-磺酸酯被用作辐射敏感性混合物中的辐射敏感成分。