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.
出处
《合成化学》
CAS
CSCD
2008年第2期230-232,共3页
Chinese Journal of Synthetic Chemistry
关键词
4
4′
4″-三硝基三苯胺
微波辐射
合成
4,4′, 4″-trinitrotriphenylamine
microware irradiation
synthesis
