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The Synthesis Of 1-Aminobenzene-4-(β-sulphatoethylsulphone)-2-sulfonic Acid

Posted on:2006-05-18Degree:MasterType:Thesis
Country:ChinaCandidate:G K HeFull Text:PDF
GTID:2121360152471816Subject:Applied Chemistry
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1-Aminobenzene-4-( β -sulphatoethylsulphone)-2-sulfonic acid is often applied to producing bifunctional-soluble reactive dyes and is an important dye intermediate. Two steps play a great role in the process of its preparation, one is chlorosulfonation reaction of acetanilide, the other is sulfonation of l-aminobenzene-4- P -sulphatoethylsulphone.The optimal reaction conditions of synthesizing p-acetanmidobenzenesufonyl chloride have been studied in the paper. In the reaction conditions, the mol ratio between acetanilide and chlorosulfonic acid is 1:3.8; the reaction temperature is 60℃; the reaction time is 2.5 hours; the usage of catalyst A is 1.6 gram. When the mol ratio between acetanilide and sulfonation agent equals 1:0.35, the mol yield is 90.24% and the productive cost is more economical; when the mol ratio between acetanilide and sulfonation agent is less than 1:0.35, the mol yield will be higher than 96.09% .l-Aminobenzene-4- β -sulphatoethylsulphone(para-ester) can be used as raw material to produce the target product l-aminobenzene-4-( β -sulphatoethylsulphone)-2-sulfonic acid through sulfonation and hydrolysis and esterification reactions. The mol yield is 89.95 % and 98.55 % on the basis of ester-group value and amino-group value respectively. The optimal reaction conditions are as follows: the mol ratio between oleum containing by weight of 50% and para-ester is 2.7:1; the addition temperature of oleum is 10-15℃; the temperature of sulfonation and hydrolysis and esterification reactions is 130 ℃ and 124℃ and 130℃ respectively, and their reaction time is 5 hours and 11.5 hours and 25 hours in turn.
Keywords/Search Tags:1 -aminobenzene-4-(- β -sulphatoethylsulphone)-2-sulfonic acid, hydrolysis l-aminobenzene-4- β -sulphatoethylsulphone (para-ester), esterification p-acetanmidobenzenesufonyl, chlorosulfonation
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