酰化反应翻译PPT课件.pptVIP

* 250 ml. of ethylene dichloride is added to the mixture. 加入250ml的二氯乙烯。 When the internal temperature has been lowered to 5°, a solution of 67 g.of freshly distilled pyrrole in 250 ml. of ethylene dichloride is added to the stirred, cooled mixture over a period of 1 hour. 当内部温度降到5度时，把67g（1.0mol）新蒸馏的吡咯加入到250二氯乙烯中，在1小时内低温下边搅拌边滴加。 * After the addition is complete, the mixture is stirred at the reflux temperature for 15 minutes。 滴加完后，加热搅拌回流15分钟。 * The mixture is then cooled to 25–30°, and to it is added a solution of 750 g.of sodium acetate trihydrate in about1:1 of water, cautiously at first, then as rapidly as possible. 当混合物降温到25-30℃后，加入750g三水醋酸钠溶液，开始要缓慢加入，然后要尽可能地快。 The reaction mixture is again refluxed for 15 minutes。 充分搅拌继续回流15分钟。 * The cooled mixture is transferred to a separatory funnel, and the ethylene dichloride layer is removed. 冷却的混合物转移到分液漏斗中，出去二氯乙烯层。 The aqueous phase is extracted three times with a total of about 500 ml. of ether. 水相用500ml乙醚分三次萃取。 * The ether and ethylene chloride solutions are combined and washed with three 100-ml. portions of saturated aqueous sodium carbonate solution. 合并乙醚和氯乙烯溶液，用100ml饱和碳酸钠溶液分三次洗涤。 * The non- aqueous solution is then dried over anhydrous sodium carbonate, the solvents are distilled, and the remaining liquid is transferred to a Claisen flask and distilled from an oil bath under reduced pressure 非水溶液用无水碳酸钠干燥，蒸馏溶剂，余下的溶液移入克氏烧瓶在油浴中减压蒸馏。 * The aldehyde boils at 78° at 2 mm Hg. 在2mmHg柱的压力下醛沸点78度。 The yield of crude 2-pyrrolealdehyde is 85–90 g. (89–95%). 粗品2-吡咯甲醛产量85-90g（89-95%）。 * The crude product is purified by dissolving in boiling petroleum ether (b.p. 40–60°), in the ratio of 1 g. of crude 2-pyrrolealdehyde to 25 ml. of solvent. 粗品溶解在沸腾的石油醚中（沸点40-60度），一克粗品2-吡咯甲醛加入25ml溶剂。 * The pure aldehyde is obtained from the crude in approximately 85% recovery.m.p. 44–45°. 纯品醛是从粗品中得到，收率85%。 熔点44-45度。 * 总的反应过程： 在三口烧瓶中加入80gDMF 冰水浴，将169g磷酰氯在15min内滴加 移去冰水浴，搅拌，加入250ml二氯乙烯 5℃时加入67g新蒸的吡咯 加热回流15min 在25-30℃