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2-氨基-4-甲氧基乙酰苯胺的合成工艺研究

         

摘要

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-me-thoxy 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 H2 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%.%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1.5 MPa,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%.

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