89-58-7 2,5-二甲基硝基苯
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安全说明
危险品运输编号1665,RTECS号ZE4686600,TSCA listed,危险等级6.1,包装类别II,海关编码29042090,毒性LD50 orl-rat: 2440 mg/kg。
用途与制备
用于有机合成;具有急性毒性(口服-大鼠LD50: 2440 毫克/公斤);与氧化剂混合可爆;明火可燃,受热分解有毒氮氧化物气体;库房通风低温干燥,与食品原料、还原剂分开储运;灭火剂为泡沫、雾状水、二氧化碳、干粉、砂土。
有机合成
产率:86.4% 合成条件:With nitric acid In acetic anhydride at 20℃; for 10 h; 实验步骤:在50mL双颈圆底烧瓶中,加入沸石HBEA-25(Si/Al=25,0.11g)、邻二甲苯(0.60mL,5mmol)、硝酸(65%,0.68mL,10mmol)和乙酸酐(5.0mL),室温搅拌反应10小时。反应结束后过滤除去沸石,滤液用NaHCO₃(3×10mL)和水(3×10mL)洗涤,有机相经无水硫酸钠干燥、过滤,得稻草黄色液体残余物。通过气相色谱内标法估算产物异构体分布和产率,柱色谱纯化后鉴定。 参考文献:[1] Russian Journal of Organic Chemistry, 1993, vol.29, #3.2, p.457-466;[2] Zhurnal Organicheskoi Khimii, 1993, vol.29, #3, p.546-558;[3] Tetrahedron Letters, 1996, vol.37, #4, p.513-516;[4] Journal of Fluorine Chemistry, 2008, vol.129, #6, p.524-528;[5] Organic Letters, 2018, vol.20, #11, p.3197-3201;[6] Green Chemistry, 2015, vol.17, #6, p.3446-3451;[7] Journal of Fluorine Chemistry, 1990, vol.46, #3, p.507-513;[8] Synthetic Communications, 2005, vol.35, #17, p.2237-2241;[9] Journal of Organic Chemistry, 2006, vol.71, #10, p.3952-3958;[10] Journal of Organic Chemistry, 1981, vol.46, #17, p.3533-3537;[11] Russian Journal of Organic Chemistry, 2005, vol.41, #10, p.1493-1495;[12] Chemische Berichte, 1997, vol.130, #5, p.581-584;[13] Bulletin of the Korean Chemical Society, 2013, vol.34, #11, p.3485-3487;[14] Chemistry Letters, 2014, vol.43, #6, p.817-819;[15] Australian Journal of Chemistry, 2015, vol.68, #7, p.1122-1128;[16] Tetrahedron Letters, 2004, vol.45, #15, p.3137-3139;[17] RSC Advances, 2013, vol.3, #3, p.691-694;[18] Journal of Organic Chemistry, 1989, vol.54, #7, p.1692-1702;[19] Journal of Organic Chemistry, 1981, vol.46, #17, p.3533-3537;[20] Journal of the American Chemical Society, 1992, vol.114, #5, p.1756-1770;[21] Journal of the American Chemical Society, 1948, vol.70, p.3787;[22] Journal fuer Praktische Chemie (Leipzig), 1935, vol.<2>142, p.153,166;[23] Justus Liebigs Annalen der Chemie, 1875, vol.176, p.55;[24] Journal of the American Chemical Society, 1953, vol.75, p.4307,4310;[25] Industrial and Engineering Chemistry, 1950, vol.42, p.352;[26] Recueil des Travaux Chimiques des Pays-Bas, 1954, vol.73, p.39,47;[27] Canadian Journal of Chemistry, 1974, vol.52, p.3960-3970;[28] Australian Journal of Chemistry, 1973, vol.26, p.775-783;[29] Journal of Organic Chemistry, 1961, vol.26, p.919-923;[30] Magnetic Resonance in Chemistry, 1985, vol.23, #7, p.597-604;[31] Journal of the Chemical Society - Perkin Transactions 2, 1995, #7, p.1541-1550;[32] Journal of the Chemical Society - Perkin Transactions 1, 1996, #19, p.2385-2389;[33] Chemical Communications, 1997, #6, p.613-614;[34] Molecules, 2005, vol.10, #8, p.978-989;[35] Advanced Synthesis and Catalysis, 2003, vol.345, #12, p.1329-1333;[36] Catalysis Communications, 2011, vol.14, #1, p.42-47;[37] Tetrahedron Letters, 2012, vol.53, #50, p.6782-6785,4;[38] Catalysis Communications, 2014, vol.49, p.82-86