化学与生物工程
化學與生物工程
화학여생물공정
CHEMISTRY & BIOENGINEERING
2014年
8期
51-53
,共3页
间二硝基苯%3-甲氧基二苯胺%乌尔曼反应%合成
間二硝基苯%3-甲氧基二苯胺%烏爾曼反應%閤成
간이초기분%3-갑양기이분알%오이만반응%합성
m-dinitrobenzene%3-methoxy diphenylamine%Ullmann reaction%sy nthesis
建立了3-甲氧基二苯胺的合成新工艺。以易得、价廉的间二硝基苯为原料，经取代、加氢还原、缩合脱水三步反应制备3-甲氧基二苯胺。确定适宜的缩合脱水反应条件为：以磷酸芳基酯为催化剂、反应原料苯酚和3-甲氧基苯胺的物质的量比为1.2∶1、反应温度为90℃、反应时间为10 h，在该条件下，缩合脱水反应收率为86.7％，总收率达到69.9％（以间二硝基苯计）。该工艺优于经典的乌尔曼合成路线，生产成本大大降低，具有很好的工业化前景。
建立瞭3-甲氧基二苯胺的閤成新工藝。以易得、價廉的間二硝基苯為原料，經取代、加氫還原、縮閤脫水三步反應製備3-甲氧基二苯胺。確定適宜的縮閤脫水反應條件為：以燐痠芳基酯為催化劑、反應原料苯酚和3-甲氧基苯胺的物質的量比為1.2∶1、反應溫度為90℃、反應時間為10 h，在該條件下，縮閤脫水反應收率為86.7％，總收率達到69.9％（以間二硝基苯計）。該工藝優于經典的烏爾曼閤成路線，生產成本大大降低，具有很好的工業化前景。
건립료3-갑양기이분알적합성신공예。이역득、개렴적간이초기분위원료，경취대、가경환원、축합탈수삼보반응제비3-갑양기이분알。학정괄의적축합탈수반응조건위：이린산방기지위최화제、반응원료분분화3-갑양기분알적물질적량비위1.2∶1、반응온도위90℃、반응시간위10 h，재해조건하，축합탈수반응수솔위86.7％，총수솔체도69.9％（이간이초기분계）。해공예우우경전적오이만합성로선，생산성본대대강저，구유흔호적공업화전경。
A novel synthetic process of 3-methoxy diphenylamine had been established.With easy and inex-pensive m-dinitrobenzene as raw material,3-methoxy diphenylamine was prepared by three-step reaction of sub-stitution,hydrogenation reduction and condensation dehydration.The optimum reaction conditions of condensa-tion dehydration were determined as follows:with aryl phosphate ester as catalyst,the molar ratio of phenol and 3-methoxy phenylamine was 1.2∶1,reaction temperature was 90 ℃,reaction time was 10 h.Under above con-ditions,the yield of the condensation dehydration was 86.7% and the total yield was 69.9%(on the basis of m-dinitrobenzene).The novel process is superior to the classic Ullmann synthetic route,greatly reduces the pro-duction cost and has good industrial prospect.
