药物合成(二).pptVIP

氯甲基化反应 The mixture is stirred while the temperature is maintained at 70±2℃ for 4-5 hours by means of a water bath .During this time hydrogen chloride is bubbled into the reaction mixture through the bent glass tube,and the excess gas is carried away through the reflux condenser to a hood or gas-absorption trap. 在水浴中保持70±2℃搅拌4-5小时，在此期间通过玻璃弯管把HCI↑通入反应混合物中，过量的气体被带到冷凝回流器被气体吸收罩吸收。 氯甲基化反应 The 2-hydroxy-5-nitrobenzyl chloride begins to separate as a solid about1 hour after the beginning of the reaction.At the end the mixture is cooled in ice for 1 hour whereby more crystals separate,after which the acid liquors are either filtered or decanted from the crystals. 在反应开始后的一个小时，2-羟基-硝基苯氯化物作为固体被分离。最后把混合物在冰中冷却一个小时，使更多的晶体析出，之后把酸性液体过滤或倾倒得到晶体。 氯甲基化反应 The 2-hydroxy-5-nitrobenzyl chloride is purified by recrystallization from 125mL of hot benzene.The yield is 46g 69% base on p-nitrophenol of a white product melting at 129-130℃。 2-羟基-硝基苯氯化物在热的苯中重结晶纯化，得白色产物46g（对硝基苯酚含69% ,熔点为129-130℃。 氯甲基化反应机理： 氯甲基化反应 氯甲基化反应 ———09药学2班第四小组制作 氯甲基化反应 In a 1L three-necked round-bottomed flask equipped with a mechanical stirrer,short reflue condenser ,and bent glass tube reaching below the surface of the liquid for the introduction of hydrogen chloride,are placed 50g 0.36mol of p-nitrophenol,650mL of concentrated hydrochloric acid,5mL of concentrated sulfuric acid,and 76g 1mol of methylal. 向配向有机械搅拌、短期冷凝回流器和一个可以深入液面下通氯化氢↑的玻璃弯管的三口圆底烧瓶中加入50g对硝基苯酚、650ml的浓盐酸、5ml的浓硫酸和76g的二甲氧基甲烷。 反应式： 谢谢聆听！ 本PPT来源于网络渠道，感谢作者的辛勤劳动，如作者不喜可私信本人删除！