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作 者:崔建兰[1] 蔡剑波[2] 曹端林[2] 邵徽旺[2] 刘璐[2]
机构地区:[1]天津大学药物科学与技术学院,天津300072 [2]中北大学化工与环境学院,山西太原030051
出 处:《合成化学》2008年第2期230-232,共3页Chinese Journal of Synthetic Chemistry
摘 要:以对硝基苯胺(1)和4-氯硝基苯(2)为原料,二甲基亚砜为溶剂,叔丁醇钾为缚酸剂,氟化钾和四甲基氯化铵为催化剂,在微波辐射下合成了4,4′,4″-三硝基三苯胺(3),其结构经IR表征。正交实验确定最佳反应条件为:13 mmol,n(1)∶n(2)∶n(叔丁醇钾)=1∶3∶2,在125 W下,于130℃反应30 min,3的收率达98.2%。4,4′, 4″-Trinitrotriphenylamine (3) was synthesized from p-nitroaniline ( 1 ) and 4-chloroni- trobenzene(2) using dimethyl sulfoxide as the solvent, potassium tert-butoxide as the antacid and the potassium fluoride and the tetramethyl ammonium chloride as the catalyst under microwave irradia- tion. The structure was confirmed by IR. The optimal reaction conditions at 130 ℃ for 30 min from orthogonal experiment were as follows: 1 was 3 mmol; n(1) : n(2) : n(potassium tert-butoxide) was 1 : 3 : 2 ; microwave power was 125 W. The yield was 98.2% under the conditions.
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