化学世界
化學世界
화학세계
CHEMICAL WORLD
2009年
10期
615-616,619
,共3页
氨基苯甲醛%Vilsmeier试剂%双(三氯甲基)碳酸酯%甲酰化
氨基苯甲醛%Vilsmeier試劑%雙(三氯甲基)碳痠酯%甲酰化
안기분갑철%Vilsmeier시제%쌍(삼록갑기)탄산지%갑선화
aminobenzaldehyde%Vilsmeier reagent%bis (trichloromethyl) carbonate%formylation
在乙酸乙酯溶剂中,以DMF和双(三氯甲基)碳酸酯(BTC)组成新的Vilsmeier试剂与N-甲基-N-取代苯胺进行甲酰化反应,合成了4-(N-甲基-N-取代)氨基苯甲醛系列化合物,一次收率达85%～90%.产品纯度超过99%.考察各类反应影响因素,确立较适宜的工艺条件:N-甲基-N-取代苯胺:DMF:BTC=1:1.2:0.4(摩尔比),反应温度75～80℃,反应时间5 h.目标化合物结构经IR与1H NMR征实.
在乙痠乙酯溶劑中,以DMF和雙(三氯甲基)碳痠酯(BTC)組成新的Vilsmeier試劑與N-甲基-N-取代苯胺進行甲酰化反應,閤成瞭4-(N-甲基-N-取代)氨基苯甲醛繫列化閤物,一次收率達85%～90%.產品純度超過99%.攷察各類反應影響因素,確立較適宜的工藝條件:N-甲基-N-取代苯胺:DMF:BTC=1:1.2:0.4(摩爾比),反應溫度75～80℃,反應時間5 h.目標化閤物結構經IR與1H NMR徵實.
재을산을지용제중,이DMF화쌍(삼록갑기)탄산지(BTC)조성신적Vilsmeier시제여N-갑기-N-취대분알진행갑선화반응,합성료4-(N-갑기-N-취대)안기분갑철계렬화합물,일차수솔체85%～90%.산품순도초과99%.고찰각류반응영향인소,학립교괄의적공예조건:N-갑기-N-취대분알:DMF:BTC=1:1.2:0.4(마이비),반응온도75～80℃,반응시간5 h.목표화합물결구경IR여1H NMR정실.
The 4-(N-methyl-N-substituted) aminobenzaldehydes were synthesized by the new Vilsmeier reaction of N-methyl-N-substituted aniline with DMF and BTC, and ethyl acetate was used as solvent. The yields of the title compounds were 85%～90% and the purity was more than 99%. The reaction conditions were optimized: mole ratio of N-methyl-N-substituted aniline : DMF : BTC=1 : 1. 2 : 0. 4, reaction temperature was 75～80 ℃, reaction time was 5 h. The structure of the products were characterized by IR and ~1H NMR spectroscopy.
