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About 216–224 g. (– moles) of powdered anhydrous aluminum chloride is added to a 1Lthree-necked -224g(– moles)的无水三***化铝。 While the free-flowing catalyst is stirred (Note 3), 81 g. ( mole) of acetophenone is added from the dropping funnel in a slow stream over a period of 20–30 minutes. 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, darkening or charring occurs. 放热反应,假如滴加的***不能被分散,就会变黑或是碳化。When about one-third of the acetophenone has been added, the mixture es a viscous ball-like mass that is difficult to ,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 addition of ketone is necessary at this point. 在这时,改用手动搅拌或快速滴加***是非常必要的。The addition of ketone, 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℃时。Near the end of the addition, the mass es molten and can be stirred easily without being either heated or cooled. The molten mass, in which the acetophenone plexed with aluminum chloride, ranges in color from tan to ,团块开始融化,表明苯乙酰已经和三***化铝混合完全,颜色也逐渐从黄褐色变为棕色。
Bromine (128 g., 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 ,熔融混合物在80-85℃蒸气浴下搅拌1小时。 plex is added in portions to a well-stirred mixture of l. of cracked ice and 100 ml. of concentrated hydrochloric acid in a 2-l. beaker (Note 6).。Part of the cold aqueous layer is added to the reaction flask to pose whatever part of the reaction mixture remains there, and the resulting mixture is added to the ,然后合并到烧杯中。 The dark oil that settles out is extracted from the mixture with four 150-ml. portions of ether 分四次把深色的油从混合物中用150ml萃取出来。The extracts bined, washed consecutively with 100 ml. of water and 100