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在酸性条件下,氯化血红素(Ⅰ)与还原性铁粉作用生成原卟啉(Ⅱ),通过HBr-冰醋酸加成不经提纯直接加入NaOH溶液,OH-取代仲位Br制得[2,7,12,18-四甲基-3,8-二(1-羟基乙基)-13,17-二羧基乙基]-卟啉(血卟啉,Ⅲ),反应总产率达到90.6%。探讨了脱铁过程中反应温度、时间、还原剂用量等因素对原卟啉(Ⅱ)合成的影响,反应时间和pH对血卟啉(Ⅲ)合成的影响。结果表明,当氯化血红素和铁粉的摩尔比为1∶1、反应温度为110℃时,原卟啉的产率最高达98.3%;当pH=10,反应时间为6 h时,血卟啉的产率最高达92.1%。通过IR、MS和1HNMR对产物结构进行了表征。
Under acidic conditions, hemin (Ⅰ) reacted with reducing iron powder to produce protoporphyrin (Ⅱ), which was directly added into NaOH solution without the addition of HBr-glacial acetic acid addition and OH-substituted secondary Br [ 2,7,12,18-tetramethyl-3,8-bis (1-hydroxyethyl) -13,17- dicarboxyethyl] -porphyrin (hematoporphyrin, Ⅲ) 90.6%. The effects of reaction temperature and time, the amount of reducing agent and other factors on the synthesis of protoporphyrin (Ⅱ) and the reaction time and pH on the synthesis of hematoporphyrin (Ⅲ) were discussed. The results showed that when the molar ratio of hemin to iron was 1: 1 and the reaction temperature was 110 ℃, the yield of protoporphyrin was up to 98.3%. When pH = 10 and reaction time was 6 h, The yield of porphyrin is up to 92.1%. The product structure was characterized by IR, MS and 1HNMR.