In a 5-l. three-necked flask mounted on a steam bath in the hood and equipped with a mechanical stirrer (Note 1) and a wide-bore condenser (Note 1) is placed 1.4 kg. (1.1 l.) of carbon disulfide. Through the open neck of the flask 202 g. (1.5 moles) of acetanilide and 300 g. (2.66 moles) of chloroacetyl chloride (Note 2) are introduced. The mixture is vigorously stirred while 600 g. (4.5 moles) of aluminum chloride is added in 25–50 g. portions over a period of 20–30 minutes; the neck of the flask is stoppered between additions (Note 3). After the addition of the last portion of aluminum chloride, the mixture is heated at reflux temperature for 30 minutes while stirring is continued. Heating and stirring are discontinued and the mixture is allowed to stand for 3 hours, during which time it separates into layers. The upper layer (carbon disulfide) is decanted, and the viscous red-brown lower layer is poured cautiously with stirring into about 1 kg. of finely crushed ice to which 100 ml. of concentrated hydrochloric acid has been added. After the hydrolysis of the aluminum chloride, the product crystallizes as a white solid, which is collected on a Büchner funnel and washed well with water. It is then transferred to a beaker where it is thoroughly washed by stirring with sufficient 95% ethanol to give a fluid slurry. The solid is again collected on the funnel. After drying in the air it melts at 213–214° and weighs 250–265 g. (79–83%). It can be recrystallized from 95% ethanol (about 1 l. of the solvent being required for 40 g. of the solid) as fine white crystals melting at 216°; the recovery in the recrystallization, without reworking of the mother liquor, is about 70%.