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1. 发明授权

US3959318A Process for preparing highly pure 5-nitro-1,4,4a,9a-tetrahydroanthraquinone 失效
标题翻译：制备高纯度5-硝基-1,4,4a，9a-四氢蒽醌的方法
公开(公告)号：US3959318A
公开(公告)日：1976-05-25
申请号：US610778
申请日：1975-09-05
申请人： Yasuyoshi Torisu , Seishichiro Kaba , Ken Mukai
发明人： Yasuyoshi Torisu , Seishichiro Kaba , Ken Mukai
IPC分类号： C07C205/47 , C07C67/00 , C07C201/00 , C07C205/45 , C07C49/68
CPC分类号： C07C201/12 , C07C205/47 , C07C221/00 , C07C2103/24
摘要： Highly pure 5-nitro-1,4,4a,9a-tetrahydroanthraquinone can be obtained by subjecting 6-nitronaphthoquinone-containing crude 5-nitro-1,4-naphthoquinone to Diels-Alder condensation reaction with 1,3-butadiene in a solvent including benzene, an alkylated aromatic hydrocarbon such as toluene, xylene or the like, a halogenated aromatic hydrocarbon such as chlorobenzene, dichlorobenzene, or the like, or a halogenated aliphathic hydrocarbon such as trichloroethylene, perchloroethylene or the like, cooling the resulting reaction solution to crystallize the reaction product, and separating the thus crystallized product by filtration. 5-nitro-1,4,4a,9a-tetrahydroanthraquinone has a relatively small solubility in the above-mentioned solvents, while the solubility of 6-nitro-1,4,4a,9a-tetrahydroanthraquinone in the solvents is rather great, thus the above-mentioned solvents being effective for the separation of these compounds from each other. The oxidation and the subsequent reduction of the thus obtained 5-nitro-1,4,4a,9a-tetrahydroanthraquinone yields 1-aminoanthraquinone with a purity above 98 wt% and a 2-aminoanthraquinone content below 1 wt%. The above-mentioned solvents are also effective for purification of 6-nitro-1,4,4a,9a-tetrahydroanthraquinone-containing 5-nitro-1,4,4a,9a-tetrahydroanthraquinone by recrystallization.
摘要翻译：通过使6-硝基萘醌的粗5-硝基-1,4-萘醌与溶剂中的1,3-丁二烯进行狄尔斯 - 阿尔德缩合反应，可以得到高纯度的5-硝基-1,4,4a，9a-四氢蒽醌包括苯，烷基化芳烃如甲苯，二甲苯等，卤代芳烃如氯苯，二氯苯等，或卤代脂族烃如三氯乙烯，全氯乙烯等，将所得反应溶液冷却至使反应产物结晶，并通过过滤分离如此结晶的产物。 5-硝基-1,4,4a，9a-四氢蒽醌在上述溶剂中的溶解度相对较小，而6-硝基-1,4,4a，9a-四氢蒽醌在溶剂中的溶解度相当大，因此上述溶剂对于将这些化合物彼此分离是有效的。由此得到的5-硝基-1,4,4a，9a-四氢蒽醌的氧化和随后的还原得到纯度高于98wt％，2-氨基蒽醌含量低于1wt％的1-氨基蒽醌。上述溶剂对于通过重结晶纯化含有6-硝基-1,4,4a，9a-四氢蒽醌的5-硝基-1,4,4a，9a-四氢蒽醌也是有效的。

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