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Çó ·­Òë  A 25 mL roundbottomed flask was charged with thiophene-2-carboxylic acid (3.5 g,4 equiv), Cu2O (1 g, 1 equiv) and toluene (12 mL).The flask was then outfitted with a Dean-Stark trap and condenser and the mixture refluxed overnight with azeotropic removal of water.The yellow/brown suspension was cooled to 60¡æ and the product was collected on a medium pore fritted-glass funnel. Under a stream of nitrogen, the filter cake was washed with methanol (12  mL) to remove excess acid, and then with ether until the eluant was colorless, and then with a small amount of hexanes. The product was dried under a flow of nitrogen, then transferred to a flask and dried further under vacuum. The product was obtained as a tan, air-stable powder that was ground with a mortar and pestle to produce a finely divided powder¡£

[ Last edited by ²î²»¶àѽѽѽ on 2015-7-24 at 09:34 ]
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