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【求助】活性染料中间体的合成
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活性染料中间体:2,3,5,6-四溴-对苯二胺,(分子式:C6H4N2Br4)合成条件方法,或者用浓盐酸溶解对苯二胺后通入溴素,需要注意哪些条件? [ Last edited by zhjf on 2008-12-10 at 17:27 ] |
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SciFinder上面可以找到一些条件 要是能找到这篇文章，估计你的问题就能解决大半了，剩下的就是条件的优化 Bibliographic Information Synthesis of maleimides based on brominated p-phenylenediamines. Gaevskii, B. D.; Markov, V. I.; Dorofeev, V. T.; Gosteminskaya, T. V. Dnepropetr. Khim.-Tekhnol. Inst., Dnepropetrovsk, USSR. Ukrainskii Khimicheskii Zhurnal (Russian Edition) (1984), 50(9), 991-5. CODEN: UKZHAU ISSN: 0041-6045. Journal written in Russian. CAN 102:131861 AN 1985:131861 CAPLUS Abstract Bromination of p-O2NC6H4NH2 gave the 2,6-dibromo deriv. which was reduced by Sn-HCl to give 84% diamine I (R = R1 = NH2). Treating the latter with maleic anhydride gave 95% I (R = HO2CCH:CHCONH, R1 = NH2) which was cyclized by Ac2O in DMF to give 90% maleimide II followed by condensation with maleic anhydride to give 85% bismaleimide III. Bromination of I (R = R1 = NH2) gave 71% of the 2,3,5,6-tetrabromo deriv. which was condensed with maleic anhydride to give 76% of the tetrabromo analog of III. The latter was also obtained in 4 steps from I (R = NO2, R1 = NH2) by condensation with maleic anhydride, redn. by Sn-HCl, bromination of the tetrachlorostannate salt, and condensation with addnl. maleic anhydride. |
3楼2008-12-10 12:38:45
2楼2008-05-29 13:36:48
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