会员体验
专利管家(专利管理)
工作空间(专利管理)
风险监控(情报监控)
数据分析(专利分析)
侵权分析(诉讼无效)
联系我们
交流群
官方交流:
QQ群: 891211   
微信请扫码    >>>
现在联系顾问~
热词
    • 8. 发明授权
    • Process for preparing highly pure
5-nitro-1,4,4a,9a-tetrahydroanthraquinone
    • 制备高纯度5-硝基-1,4,4a,9a-四氢蒽醌的方法
    • US3959318A
    • 1976-05-25
    • US610778
    • 1975-09-05
    • Yasuyoshi TorisuSeishichiro KabaKen Mukai
    • Yasuyoshi TorisuSeishichiro KabaKen Mukai
    • C07C205/47C07C67/00C07C201/00C07C205/45C07C49/68
    • C07C201/12C07C205/47C07C221/00C07C2103/24
    • 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.
    • 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。