摘要
以1-氰乙基-2-甲基咪唑(2MZCN)为原料催化氢化制备1-氨丙基-2-甲基咪唑,考察了反应过程中合成工艺参数对产物的影响,确定较为适宜的工艺条件为:温度100℃,压力5 MPa,转速624 r/min,时间4 h,溶剂是氨的饱和乙醇溶液(与原料质量比是2∶1),雷尼镍为催化剂(占原料质量的18.9%),氢氧化钾为助催化剂,原料的转化率可达99.7%,产率可达94.2%。采用红外光谱(FTIR)和核磁共振氢谱(1HNMR)及气质联用(GC-MS)对产物进行了表征。
1-Ammonia propyl-2-methyl imidazole was synthesized by catalytic hydrogenation of 1- eyanoacetate-2-methylimidazole (2MZCN), and the parameters of the synthetic process were investigated systematically in order to ascertain the appropriate synthetic conditions. The conversion of 2MZCN and the yield of 1-amino-propyl-2-methyl imidazole reached 99.7% and 94. 2% respectively after reaction for 4 h under the conditions of reaction temperature of 100 ℃ ,pressure of 5 MPa, speed of 624 r/min, and the solvent of saturated ethanol solution of ammonia( the mass ratio of the solution to the raw material is 2:1 ), Raney nickel was the catalytic agent and potassium hydroxide acted as catalyst promoter( accounting for a mass fraction of 18.9% of the raw material). The product was analysed by infrared spectroscopy(FTIR) and proton nuclear magnetic resonance spectroscopy(1HNMR) and gas chromatography-mass spectrometer( GC-MS).
出处
《精细化工》
EI
CAS
CSCD
北大核心
2013年第11期1298-1302,共5页
Fine Chemicals