新鲜铜粉“一锅法”催化Ullmann缩合反应制备4,4′-二氨基-1,1′-二蒽醌-3,3′-二磺酸钠

STUDY ON ULLMANN CONDENSATION REACTION OF PRODUCING DAS CATALYZED BY FRESH COPPER POWER IN ONE-POT METHOD

研究了用次亚磷酸钠现场液相还原硫酸铜制备新鲜铜粉,用该铜粉"一锅法"催化溴氨酸的自身Ullmann缩合反应制备4,4′-二氨基-1,1′-二蒽醌-3,3′-二磺酸钠。适宜的反应条件是:20.0g五水硫酸铜,5.8g EDTA,20.4g次亚磷酸钠,还原温度70℃,5.0g溴氨酸,缩合反应温度90℃,缩合反应时间3h,缩合产物收率可达到97.9%。

Fresh copper power directly reduced by NaH2PO2 was adopted in the Ullmann self-condensation reaction of bromamine acid to prepare 4,4＇-diamino-1,1＇-dianthraqmnonyl-3,3＇-disulfonic acid by one-pot method.Effects of condensation reaction time,condensation reaction temperature,bromamine acid dosage,concentration of CuSO4,the reduction reaction temperature on the yield of the condensation product were investigated.The condensation reaction rate monitored by thin-layer chromatography was fast.When the reaction temperature is low,bromamine acid was easily precipitated due to its low solubility.The yield of product firstly increased and then decreased with the increase of concentration of CuSO4.The optimal reaction conditions were as follows：20.0 g CuSO4 · 5H2O,5.8 g EDTA,20.4 g NaH2PO2 · H2O,reduction reaction temperature 70 ℃,5.0 g bromamine acid,condensation reaction temperature 90 ℃,condensation reaction time 3 h,the yield of the condensation product 97.9 ％.