摘要
实验以对氨基苯甲醚为原料,经酰化、硝化"一锅煮"技术制备2-硝基-4-甲氧基乙酰苯胺,2-硝基-4-甲氧基乙酰苯胺经催化还原合成2-氨基-4-甲氧基乙酰苯胺。结果表明,在90℃,n(对氨基苯甲醚)∶n(乙酸酐)=1∶1时酰化反应2h,对氨基苯甲醚转化率100%,对甲氧基乙酰苯胺选择性为99.5%。再在10℃,n(对氨基苯甲醚)∶n(发烟硝酸)=1∶1.3硝化反应2.5h,硝化过程对甲氧基乙酰苯胺转化率为99.1%,2-硝基-4-甲氧基乙酰苯胺选择性达99.8%。以雷尼镍催化剂催化加氢还原2-硝基-4-甲氧基乙酰苯胺,还原温度120℃,压力1.5MPa,m(2-硝基-4-甲氧基乙酰苯胺)∶m(催化剂)=4∶1,还原时间2h,2-硝基-4-甲氧基乙酰苯胺转化率为100%,2-氨基-4-甲氧基乙酰苯胺选择性达99.2%。
2-Amino-4-methoxy acetanilide was synthesized via the one-pot process of acetylization and nitration, and subsequent catalytic reduction using p-aminoanisole as a starting material. The results of the one-pot process showed that the conversions of p-aminoanisole and the selectivity of p-methoxy acetanilide were 100% and 99.5 %, respectively, when the acetylization reaction was carried out at 90 ℃ for 2 h with the molar ratio of p-aminoanisole to acetic anhydride of 1 ： 1. The conversion of p-methoxy acetanilide and the selectivity of 2-nitro-4-methoxy acetanilide reached 99.1% and 99.8%, respectively, when the nitration reaction was carried out at 10 ℃ for 2.5 h with the molar ratio of p- aminoanisole to nitric acid of 1 ： 1.3. When the hydrogenation of 2-nitro-4-methoxy acetanilide was catalyzed by Raney Ni catalyst at 120℃ for 2 h and Hz pressure of 1.5 MPa with the mass ratio of 2- nitro-4-methoxy acetanilide to Raney Ni catalyst of 4 ： 1, the conversion of 2-nitro-4-methoxy acetanilide reached 100 % and the selectivity of 2-amino-4-methoxy acetanilide reached 99.2 %.
出处
《精细石油化工》
CAS
CSCD
北大核心
2011年第6期34-37,共4页
Speciality Petrochemicals
