淮阴师范学院学报(自然科学版)
淮陰師範學院學報(自然科學版)
회음사범학원학보(자연과학판)
JOURNAL OF HUAIYIN TEACHERS COLLEGE (NATURAL SCIENCE EDITION)
2014年
3期
223-225,247
,共4页
方亮霞%袁文峰%支三军%韦长梅
方亮霞%袁文峰%支三軍%韋長梅
방량하%원문봉%지삼군%위장매
4-羧基苯磺酰胺%四丁基溴化铵%相转移催化%合成
4-羧基苯磺酰胺%四丁基溴化銨%相轉移催化%閤成
4-최기분광선알%사정기추화안%상전이최화%합성
4-carboxybenzenesulfonamide%tetrabutylammonium bromide%phase transfer catalysis%synthesis
研究了以水为溶剂,四丁基溴化铵( TBAB)为相转移催化剂,对甲苯磺酰胺为原料,高锰酸钾为氧化剂,合成药物中间体4-羧基苯磺酰胺的新工艺.考察了碱的用量、催化剂用量、反应温度、高锰酸钾与对甲基苯磺酰胺的摩尔比、反应时间等因素对反应收率的影响.较适宜条件为在40 mL水为溶剂,对甲基苯磺酰胺3.5 g,氢氧化钠用量为1.2 g, TBAB的用量为0.1 g,高锰酸钾与对甲基苯磺酰胺的摩尔比为2.0,反应温度70℃,反应时间2.5 h,4-羧基苯磺酰胺的产率可达93.6%.该方法具有反应条件温和、反应时间较短、操作简单和收率高等特点.
研究瞭以水為溶劑,四丁基溴化銨( TBAB)為相轉移催化劑,對甲苯磺酰胺為原料,高錳痠鉀為氧化劑,閤成藥物中間體4-羧基苯磺酰胺的新工藝.攷察瞭堿的用量、催化劑用量、反應溫度、高錳痠鉀與對甲基苯磺酰胺的摩爾比、反應時間等因素對反應收率的影響.較適宜條件為在40 mL水為溶劑,對甲基苯磺酰胺3.5 g,氫氧化鈉用量為1.2 g, TBAB的用量為0.1 g,高錳痠鉀與對甲基苯磺酰胺的摩爾比為2.0,反應溫度70℃,反應時間2.5 h,4-羧基苯磺酰胺的產率可達93.6%.該方法具有反應條件溫和、反應時間較短、操作簡單和收率高等特點.
연구료이수위용제,사정기추화안( TBAB)위상전이최화제,대갑분광선알위원료,고맹산갑위양화제,합성약물중간체4-최기분광선알적신공예.고찰료감적용량、최화제용량、반응온도、고맹산갑여대갑기분광선알적마이비、반응시간등인소대반응수솔적영향.교괄의조건위재40 mL수위용제,대갑기분광선알3.5 g,경양화납용량위1.2 g, TBAB적용량위0.1 g,고맹산갑여대갑기분광선알적마이비위2.0,반응온도70℃,반응시간2.5 h,4-최기분광선알적산솔가체93.6%.해방법구유반응조건온화、반응시간교단、조작간단화수솔고등특점.
The synthesis 4-carboxybenzenesulfonamide was investigated with TBAB as catalyst, 4-methyl-benzenesulfonamide as raw material, potassium permanganate as the oxidant and H2 O as solvent.The influen-cing factors were inspected through a series of experiments.When the mixture of 4-tolylsulfonamide 3.5 g, so-dium hydroxide 1.2 g, TBAB 0.1 g and potassium permanganate 6.5 g was stirred in 40mL water at 70℃for 2.5 h, 4-carboxybenzenesulfonamide was obtained in the yield of 93.6%.The improved method will be good industrial application prospect because of the mild reaction condition, short reaction time, excellent yield, simple operation and reduced cost.