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Òü޹ϫ: ½ð±Ò+50, ·­ÒëEPI+1, ¡ï¡ï¡ï¡ï¡ï×î¼Ñ´ð°¸ 2016-06-07 15:41:47
±¾ÎÄÒÔ 2,4-¶þÂȱ½¼×È© ºÍ ±ûͪ ΪԭÁÏ£¬Í¨¹ý ôÇÈ©ËõºÏ Éú³É4-(2,4-¶þÂȱ½»ù)-3-¶¡Ï©-2-ͪ£¬ÔÙÓë ¹ýÁ¿°±Ë® ºÏ³É Ò©ÎïÖмäÌå 7-ÂÈà­ÄÄड£¸Ã ·Ïß ½«2,4-¶þÂȱ½¼×È© Óë ¹ýÁ¿±ûͪ ÔÚ ÇâÑõ»¯ÄÆË®ÈÜÒºÖÐ µÍνÁ°è ·´Ó¦1Сʱ£¬Éú³É Öмä²úÎï 4-(2,4-¶þÂȱ½»ù)-3-¶¡Ï©-2-ͪ¡£ÔÚ ´ß»¯¼Á Ñõ»¯ÑÇÍ­µÄ ´ß»¯Ï£¬ÒÔ ¶þ¼×»ù¼×õ£°· ×÷ÈܼÁ ÔÚ100 ¡æÏ ·´Ó¦12Сʱ£¬µÃ Ä¿±ê²úÎï 7-ÂÈà­ÄÄड£Í¨¹ý µ÷½Ú Ô­ÁÏĦ¶û±È¡¢·´Ó¦ÎÂ¶È ÒÔ¼° ·´Ó¦Ê±¼ä µÈÒòËØ£¬Ì½¾¿ 7-ÂÈà­ÄÄà¤µÄ ×î¼ÑºÏ³ÉÌõ¼þ£¬ÊÕÂÊ ¿É´ï66.57%¡£Í¨¹ý ºìÍâ¹âÆ×¡¢ÖÊÆ×µÈ ±íÕ÷ÊÖ¶Î ¶Ô²úÎï ½øÐбíÕ÷¡£¸Ã·Ïß °²È«ÐԸߡ¢²Ù×÷ÐÔÇ¿£¬ÓÐÒ»¶¨µÄ ¹¤Òµ»¯Ç°¾°¡£
In this paper, based on 2,4-dichlorobenzaldehyde and acetone as raw material, 4-(2,4-dichlorophenyl)-3-butene-2-ketone was first synthesized by method of aldol condensation, and then the drug intermediate-7-Chloro quinaldine was prepared by adding excessive amount of ammonia liquor. By this approach, 2,4-dichlorobenzaldehyde and excessive acetone were subjected to cold mixing in sodium hydroxide solution for 1 h, so that the intermediate product- 4-(2,4-dichlorophenyl)-3-butene-2-ketone can be prepared. Catalyzed by cuprous oxide, reaction was kept at 100 ¡æ for 12 h, in which dimethylformamide served as solvent, and thus target product 7-Chloro quinaldine can be obtained. Through adjusting factors such as molar ratio of raw material, reaction temperature, and reaction time, this research explored the optimum synthesis condition of 7-Chloro quinaldine, and found that yield coefficient can reach 66.57%. By characterizing the resulted products using infrared spectroscopy and mass spectrum, it demonstrated that such approach was superior for its higher safety and operability, and of certain prospect of industrialization application.
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