Produccce Hie Lo Ajo

1. Procedure
In a 5-l. two-necked, round-bottomed flask fitted with a good mechanical stirrer (Note 1), a separatory funnel, a thermometer,and a reflux condenser connected with a trap (Note 2) for absorbing the hydrogen chloride evolved, are placed 455 g. (3.4 moles) ofanhydrous aluminum chloride (Note 3) and 1 l. (10.2 moles) of dry carbon tetrachloride (Note 4). The flask is surrounded by an ice bath (Note 5). Thestirrer is started and when the temperature of the carbon tetrachloride has dropped to 10–15°, 50 cc. of dry thiophene-free benzene (Note 6)is added all at once. The reaction begins immediately as is indicated by the evolution of hydrogen chloride and a rising temperature. Assoon as the reaction has started, salt is added to the ice in the cooling bath in order to get more effective cooling. When the temperaturebegins to fall after the reaction has started, a mixture of 550 cc. (a total of 6.7 moles) of thiophene-free benzene and 550 cc. (a total of 14.5moles) of carbon tetrachloride is run in at such a rate that the temperature is kept between 5° and 10° (Note 5). If efficient cooling ismaintained, this addition requires one to two hours. The stirring is continued for about three hours after the benzene-carbon tetrachloridesolution has been added, while the temperature is held at about 10°. The stirring is then discontinued and the mixture is allowed to stand about