- Synthetic Approach of Triphenylaluminum
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Triphenyl (CAS NO.: ), with other names as Aluminum, triphenyl-, could be produced through the following synthetic routes.
A 500-ml. one-necked flask with a side arm to admit nitrogen is fitted with a reflux condenser protected at the top by a T-tube through which nitrogen is slowly passed during the entire reaction. In the flask there is placed 12 g. (0.44 g. atom) of aluminum wool, and the system is thoroughly dried by flaming and then cooled to room temperature. A positive pressure of nitrogen is maintained in the system by admission of the gas through the side arm while the flask is detached from the condenser, stoppered, and transferred to a nitrogen-filled dry box. To the flask there is added 80 g. (0.23 mole) of diphenylmercury which is spread evenly on top of the aluminum wool, followed by 340 ml. of sodium-dried xylene. The flask is stoppered, returned to the condenser, and immersed in a preheated oil bath, which is maintained at 140–150°. The reaction mixture is allowed to reflux for 24 hours, the water drained from the condenser, and the top of the condenser is connected to a vacuum system through a trap cooled in dry ice. The xylene is distilled by gradually reducing the pressure to 20–30 mm. The flask is cooled to room temperature and nitrogen readmitted.
The flask is returned to the dry box, and the nearly dry solid that remains in it is transferred to an extraction thimble (123 mm. × 43 mm.) previously dried in a vacuum oven. The product is extracted in a dried Soxhlet apparatus (250 mm. × 50 mm.) with 250 ml. of dry ether in a carefully dried 300-ml. flask. The extraction is continued for 15–20 hours, during which time white crystals of triphenylaluminum etherate form in the flask. The flask and its contents are placed in a dry box, the ether is decanted, and the crystals are washed several times by decantation with small portions of dry ether. The triphenylaluminum etherate is dried at 25° under reduced pressure; m.p. 126–130°. The ether of crystallization is removed by heating the etherate at 150° (0.1 mm.) for about 13 hours. Pure triphenylaluminum, m.p. 229–232°, is obtained; yield 23–27 g. (59–70%).
Notice: Triphenylaluminum and its etherate undergo decomposition in the presence of air and moisture. Upon contact with water, vigorous heat evolution and sparking have been observed.
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