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°®ÓëÓêÏÂ: ½ð±Ò+1 2012-06-07 19:24:23
dcjb: ½ð±Ò+140, ·­ÒëEPI+1, ¡ï¡ï¡ïºÜÓаïÖú, ·­ÒëµÃ²»´í£¬ÊµÑé·­Òë³É¹ýȥʽµÄ¾Í¸üºÃÁË£¬²»¹ý¹ÖÎÒû˵Çå³þ 2012-06-09 12:45:56
Add 9.5mL£¨0.2mol£©anhydrous ethanol and 6mL (0.10mol) acetic acid into a 50mL round bottom flask£¬and then add carefully 2.5mL concentrated sulphuric acid. After mixing thoroughly£¬add zeolites and install condensation tubes.
Carefully heat the reaction flask to maintain a slow reflow during 1/2 h. After the reactants in the flask are cooled down£¬the reflow device are changed into the distillation apparatus and the receiving flask is cooled down using cold water. Heat the ethyl acetate generated by steam, until the volume of distillate liquid is about 1/2 of the total volume of reactants.
Slowly add the saturated sodium carbonate solution into the distillate liquid, with continuous stirring£¬until there is no generation of carbon dioxide gas. Then transfer the mixture to a separatory funnel and remove the aqueous solution in the lower layer. The organic layer is washed with 5mL saturated salt water£¬followed by 5mL saturated calcium chloride solution and finally with water£¬and the lower liquid is removed. The organic layer is transferred into a dry triangular flask£¬and is dried using anhydrous magnesium sulfate£¬which produces a crude product about 6.8g. Distill the dried organic layer and collect the fraction of 73 ~ 78 ¡ã C, with a final production about 4.2g.

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