文档介绍：大连理工大学硕士学摄论文攘要 “对位酯”,是合成KN激、M型活性染料的中闻体,是乙烯砜型染料媛重要昀活悭簇之一。本论文黪王作主要鸯两方葱: 1、用文献己经报道的硫醚氧化法食成对位酯,对取代还原粕缩合两步反成进行改进,改进后的工艺简单,反成时间短,收率由文献报道的83%提高到88‘3%,纯度98+69%, 从瑟降馁了您产戆成本。以慰磷茎氯攀为蒙瓣,曩麓纯镳取代还灏,与氯乙醇缀合,再用双氧永氧化,后与浓硫酸酯化得到对像酯。所得结果: :1,反应温胰104~106℃,反应时问7h,5d DMSO,反威完后调pH德歪8,对氨纂苯硫酚的收率为85。2%。 b嚣台爱瘟::l,室温下爱疲4小对,p融8~9, %。 :双氧水、:1:,在 50~60"C,发应孛控裁p薹薹馕5。5~6,5,爱应簿翅4,5h,对氨基苯慕,§%。 :初步考察了稀释的水量对对位酯收率的影响,%, %,酯值96,47%。 2、设诗了一条薮瓣合成对谴酯静爨线: ,13,,再经氧化制备对位酯。对耘约会成蹙线终了裙步兹除段蠼窳验磅究。爨褥缝莱:8,:l,反应时间2h,在109C戳下,8。氯乙醇硫酸酯钠盐的牧率为95%。-。并在此基础上初步考察了以水作溶剂时,。霹奉交夸合藏懿孛阗产锈、最终产魏及荬毽程关讫合秘逶行了绫梅表{歪。论文对对位酯的合成研究所得结论,为对位酯的工业化生产提供了工艺改谶的依据。美键词;对位穗;活性染_j|罨;对氨基苯硫酚:§一氯己簿硫酸跨 4, Researches on synthesis of4一aminophenyl一§一sutfatoethylsulfone Abstract. -sulfatoethylsulfone(abbr。as p-ester)is allimportant synthetic intermediateofKN-type andM—type reactive dyes,and themost important reactive group of vinyl—Sulfone reactivedyes. 嚣豫experimental part&the thesiscontains two aspects: of4一aminophenyl一8一sulfatoethylsulfone carlbe seen insome literatures, and condensation,after optimization theprocess issimple,effectively reduce increase theyield from 83%reported by literature %,purity at %,so reduced the COSt。#一AminophenyI一13一sulfatoethylsulfone was prepared from ,followed by thefoursteps:substitution-reduction by sodium sulfide, condensation withchloroethanol,the oxidation by hydrogen peroxide,then etherification by concenlrated sulfuric acid toobtainP- following results are gained: a。露le molar ratio ofsodium sulfide and p-nitrochlorobenzene :1,the reaction temperature ℃for 7hours,5dDMSO,after the reaction isover,thenadjust thepH