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    • 42. 发明授权
    • Process for the preparation of 1-amino-2-ethoxy-naphthalene-6-sulphonic
acid
    • 制备1-氨基-2-乙氧基 - 萘-6-磺酸的方法
    • US4341719A
    • 1982-07-27
    • US238327
    • 1981-02-26
    • Rolf PutterTheodor PfisterManfred NiesePeter Wenzl
    • Rolf PutterTheodor PfisterManfred NiesePeter Wenzl
    • C07C309/50C07C67/00C07C301/00C07C303/02C07C303/22C07C309/47C07C143/66
    • C07C309/00
    • A process for the preparation of 1-amino-2-ethoxy-naphthalene-6-sulphonic acid from 2-hydroxy-naphthalene-6-sulphonic acid which comprises:A. contacting 2-hydroxy-naphthalene-6-sulphonic acid with at least an equimolar amount of an alkali metal nitrite in aqueous solution or suspension in the presence of hydrochloric acid, solution or suspension having a pH in the range of 2 to 5 and being at a temperature of 0.degree. to 20.degree. C.;B. reducing the reaction product of step A in an aqueous suspension by contacting the same with excess iron in the presence of at least an equivalent amount of iron-II ions, relative to the reaction product obtained according to step A, in the presence of a mineral acid at a temperature from 50.degree. to 120.degree. C., and treating the thus-obtained reaction mixture with aqueous alkali metal hydroxide in the presence of iron oxide;C. contacting the product of step B with excess acetic anhydride in an aqueous solution or suspension at a pH in the range of 3 to 10 at a temperature from 0.degree. to 100.degree. C.;D. contacting the product of step C with an ethylating agent in the presence of an acid binding agent in an aqueous-organic solvent or diluent in a pH range from 8 to 14 at a temperature from 20.degree. to 150.degree. C.; andE. deacetylating the product of step D by contacting the same at reflux with an aqueous alkali metal hydroxide.
    • 一种从2-羟基 - 萘-6-磺酸制备1-氨基-2-乙氧基 - 萘-6-磺酸的方法,其包括:A.将2-羟基 - 萘-6-磺酸与至少 在盐酸,溶液或悬浮液的存在下,在pH为2至5,温度为0至20℃的水溶液或悬浮液中,等摩尔量的碱金属亚硝酸盐。 B.通过在相对于根据步骤A获得的反应产物存在下,在至少相当量的铁-II离子的存在下,使其与过量的铁接触,将步骤A的反应产物还原在水性悬浮液中 在50〜120℃的温度下进行无机酸处理,在氧化铁存在下用碱金属氢氧化物水溶液处理得到的反应混合物; C.将步骤B的产物与过量的乙酸酐在0至100℃的温度下,在3至10的pH范围内的水溶液或悬浮液中接触。 D.在酸性粘合剂存在下,在pH范围为8-14的含水有机溶剂或稀释剂中,在20-150℃的温度下,使步骤C的产物与乙基化剂接触。 和E.通过使其与碱金属氢氧化物水溶液在回流下使其脱离乙酰化步骤D的产物。