摘要
以3-氟甲苯为原料,用三种不同硝化反应制备了5-氟-2-硝基甲苯.采用混酸硝化(在溶剂中,36.2ml浓硝酸、14.8ml浓硫酸、0℃～5℃、90g 3-氟甲苯),5-氟-2-硝基甲苯的选择性为59.8%;68%的浓硝酸/多聚磷酸硝化(28.0ml 68%硝酸、0℃～5℃、35g多聚磷酸、16.5g 3-氟甲苯)5-氟-2-硝基甲苯的选择性为80.0%;浓硝酸硝化(96.5ml浓硝酸、200g 3-氟甲苯、50℃～55℃、8小时、真空蒸馏)5-氟-2-硝基甲苯的选择性为79.9%,应用H-MR和IR对产品进行了表征.
5-Fluoro-2-nitro-toluene was prepared from 3-fluorotoluene by three nitration processes: (1) nitration with mixed acid of HNO3-H2SO4 (in solvent, 36.2ml concentrated sulfuric acid, 14.8ml concentrated nitric acid, 0-5 V., 90g 3-fluorotoluene) giving a selectivity of 59.8% for 5-fluoro-2-nitro-toluene; (2) with mixed acid of 68%HNO3-H3PO4 (28.0ml 68% nitric acid, 0-51:, 35g polyphosphoric acid, 16.5g 3-fluorotoluene) giving a selectivity of 80.0%; (3) with concentrated nitric acid (96.5ml concentrated nitric acid, 200g 3-fluorotoluene, 50-55 ℃, 8 hours, distilled under vacuum) giving a selectivity of 79.9%. The product was characterized by 1H-NMR and IR.
出处
《染料与染色》
CAS
2004年第5期271-273,共3页
Dyestuffs and Coloration
