公开(公告)号：US4490562A

公开(公告)日：1984-12-25

申请号：US462258

申请日：1983-01-31

申请人： Werner Schreiber ,  Michael Marky

发明人： Werner Schreiber ,  Michael Marky

IPC分类号： C07C41/30 ,  C07C41/00 ,  C07C41/26 ,  C07C41/34 ,  C07C41/40 ,  C07C43/295 ,  C07C67/00 ,  C07C41/38 ,  C07C41/42

CPC分类号： C07C41/26 ,  C07C41/38 ,  C07C41/40

摘要： A very pure, dust-free commercial form of 4,2',4'-trichloro-2-hydroxydiphenyl ether with little odor is prepared by diazotizing 4,2'4'-trichloro-2-aminodiphenyl ether, boiling the diazonium salt and purifying the reaction product. The pure, dust-free and odor-free commercial form is obtained by separating off the acid aqueous phase of the reaction mixture, rendering the mixture containing 4,2'4'-trichloro-2-hydroxydiphenyl ether and 2,4,8-trichlorodibenzofuran alkaline, extracting it several times with an inert water-immiscible solvent, either after removal of the organic solvent by steam distillation and precipitation of the by-product 2,4,8-trichlorodibenzofuran or directly, and then adjusting the pH to 3 to 10; subsequently, the highly volatile constituents are removed from the 4,2',4'-trichloro-2-hydroxydiphenyl ether melt which has separated out, the melt is subjected to molecular distillation and the distilled melt is introduced into an aqueous dispersion of crystalline 4,2',4'-trichloro-2-hydroxydiphenyl ether, this dispersion simultaneously being subjected to wet grinding. Filtration and drying gives a granular-like ready-to-use commercial form.

摘要翻译： 通过重氮化4,2'4'-三氯-2-氨基二苯醚，沸腾重氮盐和重氮化物制备非常纯净，无尘的商业形式的4,2'，4'-三氯-2-羟基二苯醚， 纯化反应产物。 通过分离出反应混合物的酸性水相，得到纯的无尘，无臭味的商业形式，使含有4,2'-四氯-2-羟基二苯醚和2,4,8-三氯-2-羟基二苯醚的混合物， 三氯二苯并呋喃碱性，用惰性水不混溶溶剂萃取数次，无论是通过蒸汽蒸馏除去有机溶剂并沉淀副产物2,4,8-三氯二苯并呋喃或直接，然后将pH调节至3〜 10; 随后，从分离出的4,2'，4'-三氯-2-羟基二苯醚熔体中除去高挥发性成分，熔融物进行分子蒸馏，将蒸馏的熔体引入结晶4的水分散体 ，2'，4'-三氯-2-羟基二苯醚，该分散体同时进行湿磨。 过滤和干燥得到颗粒状的即用型商业形式。

公开(公告)号：US4390476A

公开(公告)日：1983-06-28

申请号：US318647

申请日：1981-11-05

申请人： Michael Marky

发明人： Michael Marky

IPC分类号： C07F9/54 ,  C07C145/00 ,  C07C63/36 ,  C07C143/38

CPC分类号： C07F9/54

摘要： Phosphonium compounds of the formula(R).sub.3 P.sup..sym. --CH.sub.2 --X--CH.dbd.CH--R.sub.1 --Y.sup..crclbar.in which R is preferably alkyl having 1 to 4 C atoms, cyclohexyl or phenyl, R.sub.1 is a substituted or unsubstituted aromatic radical, especially a phenyl radical, X is phenylene, 4,4'-biphenylene or 1,4- or 2,6-naphthylene and Y.sup..crclbar. is SO.sub.3.sup..crclbar., SO.sub.2.sup..crclbar. or COO.sup..crclbar., a process for their preparation and a process for the preparation of asymetrically substituted fluorescent brightening agents of the formulaZ--CH.dbd.CH--X--CH.dbd.CH--R.sub.1 --Y.sup..crclbar. M.sup..sym.in which R.sub.1, X and Y.sup..crclbar. are as defined above, M.sup..sym. is a cation and Z is preferably a substituted or unsubstituted phenyl or 2-phenyl-triazol-4-yl radical, by reacting a bis-phosphonium compound of the formula ##STR1## in which Q.sup..crclbar. is an anion, with an aldehyde of the formula M.sup..sym. Y.sup..crclbar. --R.sub.1 --CHO and reacting the resulting intermediate with an aldehyde of the formula Z--CHO.

摘要翻译： 式（R）3P（+） - CH2-X-CH = CH-R1-Y（ - ）的鏻化合物，其中R优选为具有1至4个C原子的烷基，环己基或苯基，R 1为取代或未取代的 芳基，特别是苯基，X是亚苯基，4,4'-亚联苯基或1,4-或2,6-亚萘基，Y（ - ）是SO 3（ - ），SO 2（ - ）或COO（ - ）， 其制备方法和制备式Z-CH = CH-X-CH = CH-R 1 -Y（ - ）M（+）的非对称取代荧光增白剂的方法，其中R 1，X和Y（ - ）如上所定义，M（+）​​是阳离子，并且Z优选为取代或未取代的苯基或2-苯基 - 三唑-4-基，通过使式“IMAGE”的双鏻化合物与 Q（ - ）是具有式M（+）Y（ - ） - R1-CHO的醛的阴离子，并使得到的中间体与式Z-CHO的醛反应。

公开(公告)号：US4316860A

公开(公告)日：1982-02-23

申请号：US150026

申请日：1980-05-15

申请人： Michael Marky

发明人： Michael Marky

IPC分类号： C07C309/32 ,  C07D249/06 ,  C07D317/56 ,  C07D319/08 ,  C07F9/54 ,  C09B57/00 ,  C11D1/00 ,  C07C145/00 ,  C07C63/36 ,  C07C143/38

CPC分类号： C07D319/08 ,  C07C309/00 ,  C07D249/06 ,  C07D317/56 ,  C07F9/5449 ,  C07F9/5456

摘要： Phosphonium compounds of the formula(R).sub.3 P.sup..sym. --CH.sub.2 --X--CH.dbd.CH--R.sub.1 --Y.sup..crclbar.in which R is preferably alkyl having 1 to 4 C atoms, cyclohexyl or phenyl, R.sub.1 is a substituted or unsubstituted aromatic radical, especially a phenyl radical, X is phenylene, 4,4'-biphenylene or 1,4- or 2,6-naphthylene and Y.sup..crclbar. is SO.sub.3.sup..crclbar., SO.sub.2.sup..crclbar. or COO.sup..crclbar., a process for their preparation and a process for the preparation of asymetrically substituted fluorescent brightening agents of the formulaZ--CH.dbd.CH--X--CH.dbd.CH--R.sub.1 Y.sup..crclbar. M.sup..sym.in which R.sub.1, X and Y.sup..crclbar. are as defined above, M.sup.61 is a cation and Z is preferably a substituted or unsubstituted phenyl or 2-phenyl-triazol-4-yl radical, by reacting a bis-phosphonium compound of the formula ##STR1## in which Q.sup..crclbar. is an anion, with an aldehyde of the formula M.sup..sym. Y.sup..crclbar. --R.sub.1 --CHO and reacting the resulting intermediate with an aldehyde of the formula Z--CHO.

摘要翻译： 式（R）3P（+） - CH2-X-CH = CH-R1-Y（ - ）的鏻化合物，其中R优选为具有1至4个C原子的烷基，环己基或苯基，R 1为取代或未取代的 芳基，特别是苯基，X是亚苯基，4,4'-亚联苯基或1,4-或2,6-亚萘基，Y（ - ）是SO 3（ - ），SO 2（ - ）或COO（ - ）， 其制备方法和制备式Z-CH = CH-X-CH = CH-R 1 Y（ - ）M（+）的非对称取代的荧光增白剂的方法，其中R1，X和Y（ - ） M61是阳离子，Z优选为取代或未取代的苯基或2-苯基 - 三唑-4-基，其中Q（ - ）为 阴离子，与式M（+）Y（ - ） - R1-CHO的醛反应，并使得到的中间体与式Z-CHO的醛反应。

公开(公告)号：US4231957A

公开(公告)日：1980-11-04

申请号：US950902

申请日：1978-10-12

申请人： Michael Marky

发明人： Michael Marky

IPC分类号： C07C309/32 ,  C07D249/06 ,  C07D317/56 ,  C07D319/08 ,  C07F9/54 ,  C09B57/00 ,  C11D1/00 ,  C07C143/24 ,  D06P1/38

CPC分类号： C07D319/08 ,  C07C309/00 ,  C07D249/06 ,  C07D317/56 ,  C07F9/5449 ,  C07F9/5456

摘要： Phosphonium compounds of the formula(R).sub.3 P.sup..sym. --CH.sub.2 --X--CH.dbd.CH--R.sub.1 Y.sup..crclbar.in which R is preferably alkyl having 1 to 4 C atoms, cyclohexyl or phenyl, R.sub.1 is a substituted or unsubstituted aromatic radical, especially a phenyl radical, X is phenylene, 4,4'-biphenylene or 1,4- or 2,6-naphthylene and Y.sup..crclbar. is SO.sub.3.sup..crclbar., SO.sub.2.sup..crclbar. or COO.sup..crclbar., a process for their preparation and a process for the preparation of asymetrically substituted fluorescent brightening agents of the formulaZ--CH.dbd.CH--X--CH.dbd.CH--R.sub.1 --Y.sup..crclbar. M.sup..sym.in which R.sub.1, X and Y.sup..crclbar. are as defined above, M.sup..sym. is a cation and Z is preferably a substituted or unsubstituted phenyl or 2-phenyl-triazol-4-yl radical, by reacting a bis-phosphonium compound of the formula ##STR1## in which Q.sup..crclbar. is an anion, with an aldehyde of the formula M.sup..sym. Y.sup..crclbar. --R.sub.1 --CHO and reacting the resulting intermediate with an aldehyde of the formula Z--CHO.

摘要翻译： 式（R）3P（+） - CH2-X-CH = CH-R1Y（ - ）的鏻化合物，其中R优选为具有1至4个C原子的烷基，环己基或苯基，R 1为取代或未取代的芳族基团 特别是苯基，X是亚苯基，4,4'-亚联苯基或1,4-或2,6-亚萘基，Y（ - ）是SO 3（ - ），SO 2（ - ）或COO（ - ）， 其制备方法和制备式Z-CH = CH-X-CH = CH-R 1 -Y（ - ）M（+）的不对称取代的荧光增白剂的方法，其中R1，X和Y（ - ） 如上定义，M（+）​​是阳离子，Z优选为取代或未取代的苯基或2-苯基 - 三唑-4-基，通过使式（IMAGE）的双鏻化合物与Q（ - ）是具有式M（+）Y（ - ） - R1-CHO的醛的阴离子，并使得到的中间体与式Z-CHO的醛反应。