化学研究与应用
化學研究與應用
화학연구여응용
CHEMICAL RESEARCH AND APPLICATION
2007年
11期
1282-1284
,共3页
吴志兵%宋保风%李瑛%李龙章%蒋青
吳誌兵%宋保風%李瑛%李龍章%蔣青
오지병%송보풍%리영%리룡장%장청
合成%硝基甲烷%三羟甲基氨基甲烷%缩合
閤成%硝基甲烷%三羥甲基氨基甲烷%縮閤
합성%초기갑완%삼간갑기안기갑완%축합
synthesis%nitromethane%tris-(hydroxymethyl)-aminomethane%condensation
通过对羟甲基化反应条件的研究,找出了有效提高合成三羟甲基硝基甲烷产率的方法,即n(硝基甲烷)∶ n(甲醛)= 1∶ 3.2,Ca(OH)2溶液作催化剂,调节pH值至9左右,控温30℃反应4小时,得到三羟甲基硝基甲烷,产率达91.3%.在乙醇和二氯甲烷的溶剂中以水合肼为还原剂,加入催化剂还原硝基.将还原芳香族硝基化合物的方法应用到多羟基脂肪族硝基化合物上.
通過對羥甲基化反應條件的研究,找齣瞭有效提高閤成三羥甲基硝基甲烷產率的方法,即n(硝基甲烷)∶ n(甲醛)= 1∶ 3.2,Ca(OH)2溶液作催化劑,調節pH值至9左右,控溫30℃反應4小時,得到三羥甲基硝基甲烷,產率達91.3%.在乙醇和二氯甲烷的溶劑中以水閤肼為還原劑,加入催化劑還原硝基.將還原芳香族硝基化閤物的方法應用到多羥基脂肪族硝基化閤物上.
통과대간갑기화반응조건적연구,조출료유효제고합성삼간갑기초기갑완산솔적방법,즉n(초기갑완)∶ n(갑철)= 1∶ 3.2,Ca(OH)2용액작최화제,조절pH치지9좌우,공온30℃반응4소시,득도삼간갑기초기갑완,산솔체91.3%.재을순화이록갑완적용제중이수합정위환원제,가입최화제환원초기.장환원방향족초기화합물적방법응용도다간기지방족초기화합물상.
A effective synthetic method for tris-(hydroxymethyl)-nitromethane was reported under the reacting condition of n (nitromethane): n (formaldehyde)=1∶ 3.2,calcium hydroxide as the catalyst,pH9 and stirred at 30℃ 4 h was describe,the yield got 91.3%. Another new attempt about using the method of deoxidizing nitro aromatic compounds to reduce the nitro acyclic compounds which with polyhydric alcohols was made,and the yield of the tris-(hydroxymethyl)-aminomethane got 50%.