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    • 22. 发明授权
    • Process for preparation of
3-(acyl)amino-4-alkoxy-phenyl-.beta.-hydroxyethyl-sulfone (sulfonates)
    • 制备3-(酰基)氨基-4-烷氧基 - 苯基-β-羟基乙基砜(磺酸盐)的方法
    • US4778911A
    • 1988-10-18
    • US065678
    • 1987-06-18
    • Peter HessFolker KohlhaasTheodor Papenfuhs
    • Peter HessFolker KohlhaasTheodor Papenfuhs
    • C07C315/00C07C67/00C07C313/00C07C315/04C07C317/36C07C317/40C07C141/16C07C103/127C07C103/22
    • C07C315/00
    • A process for the preparation of 3-(acyl)amino-4-alkoxy-phenyl-.beta.-hydroxyethyl-sulfone (sulfates) of the formula (1) ##STR1## in which R.sub.1 is alkyl having 1-4 carbon atoms and R.sub.2 is hydrogen or one of the groupings ##STR2## with the proviso that n=1 if R.sub.2 =H and n=0 if R.sub.2 =acyl, by converting 2-alkoxyacylanilines of the formula (2) ##STR3## in which R.sub.1 and R.sub.2 have the meanings given, in a known manner to the corresponding sulfochlorides substituted in the p-position relative to the alkoxy group, reducing the sulfochlorides with an alkali metal sulfite or ammonium sulfite in an aqueous medium at pH 7.0-8.5 and at -5 to +40.degree. C. to give the corresponding sulfinates, alkoxylating the latter with ethylene oxide in an aqueous medium at pH 6.0-8.5 and 40.degree.-80.degree. C. to give the 3-acylamino-4-alkoxyphenyl-.beta.-hydroxyethyl-sulfones of the formula (1) (with R.sub.2 =acyl and n=0) and, if appropriate, esterifying the latter, with deacylation, with concentrated sulfuric acid at 70.degree.-150.degree. C. to give the compounds of the said formula (1) (with R.sub.2 H and n=1).
    • 制备式(1)的3-(酰基)氨基-4-烷氧基 - 苯基-β-羟基乙基砜(硫酸盐)的方法其中R1是具有1-4个碳原子的烷基 并且R2是氢或分组 + TR ,条件是如果R2 = H,n = 1,如果R2 =酰基,则n = 0,通过将2-烷氧基苯甲酰苯胺 式(2)其中R 1和R 2具有已知方式给予在相对于烷氧基的p位取代的对应的磺基氯的含义,用碱金属亚硫酸盐或铵还原磺酰氯 亚硫酸盐在pH 7.0-8.5和-5至+ 40℃的水性介质中,得到相应的亚硫酸盐,将其与环氧乙烷在pH 6.0-8.5和40 -80℃的水性介质中烷氧基化成 得到式(1)的3-酰基氨基-4-烷氧基苯基-β-羟乙基砜(R2 =酰基和n = 0),并且如果合适的话,将后者酯化,用去酰基化,浓缩 硫酸在70-150℃,得到所述式(1)的化合物(其中R2H和n = 1)。