药物合成反应(闻韧第三版)课后翻译.docxVIP

1、 About 216 -224 g. (1.62 —.68 moles) of powdered an hydrous alumi num chloride is added to a 1Lthree-necked flask. 在 1L 的三口烧瓶中加入大约 216-224g(1.62 —.68 moles) 的无水三氯化铝。 While the free-flowi ng catalyst is stirred (Note 3), 81 g. (0.67 mole) of acetophe none is added from the dropp ing funnel in a slow stream over a period of 20 -30 min utes. 自由流动的催化剂边搅拌边用 滴液漏斗缓慢滴加 81g 苯乙酰。Considerable heat is evolved, and, if the drops of ketone are not dispersed, darke ning or charri ng occurs. 放热反应，假如滴加的酮不能被分散， 就会变黑或是碳化。 When about on e-third of the acetophe none has bee n added, the mixture becomes a viscous ball-like mass that is difficult to stir. 当三分之一的乙酰苯 被滴加，反应混合物变成一个很难搅拌的粘性的球状团块。 Turning of the stirrer by hand or more rapid additi on of ket one is n ecessary at this point. 在这时，改用手动搅拌或快速 滴加酮是非常必要的。 The additi on of ket one, however, should not be so rapid as to produce a temperature above 180 .然而，速度不能太快，当反应温度超过 180 C时。 Near the end of the additi on, the mass becomes molte n and can be stirred easily without being either heated or cooled. The molte n mass, in which the acetophe none is complexed with alumi num chloride, ran ges in color from tan to brow n. 当快滴加完 时，团块开始融化，表明苯乙酰已经和三氯化铝混合完全，颜色也逐渐从黄褐色变为棕色。 Bromine (128 g., 0.80 mole) is added dropwise to the well-stirred mixture over a period of 40 minutes (Note 4). 在40分钟内在搅拌下把溴缓慢滴加到混合物中。 After all the bromine has been added, the molten mixture is stirred at 80 —85 ° on a steam bath for 1 hour. 溴滴加完后，熔融混合物在 80-85 C蒸气浴下搅拌 1小时。The complex is added in portions to a well-stirred mixture of 1.3 l. of cracked ice and 100 ml. of concentrated hydrochloric acid in a 2-l. beaker (Note 6). 反应物加入到 1.3L 碎冰和 100ml 浓盐酸的混合物中在 2L的烧杯中混合均匀。Part of the cold aqueous layer is added to the reacti on flask to decompose whatever part of the reacti on mixture remai ns there, and the resulti ng mixture is added to the beaker. 把部分的冰水层加入到烧瓶中 洗涤残留物，然后合并到烧杯中。 The dark oil that settles out is extracted from the mixture with four 150-ml. portio ns of ether 分四次把