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ÖØ½á¾§£º½«227.3gÎö¾§Â˱ý¼ÓÈëµ½2L¸ÉÔïµÄËÄ¿ÚÉÕÆ¿ÖУ¬¼ÓÈë454.6gTHF£¬ÉýÎÂÖÁ60-65¡æ£¬Ê¹¹ÌÌåÍêÈ«Èܽ⣬±£ÎÂ10min£¬ºó½µÎÂÖÁ50¡æÓý¾§1h£¬½µÎÂÖÁ-15~ -10¡æ±£ÎÂ1h£¬¹ýÂ˵ÃÂ˱ý219.12g£¬HPLC´¿¶È99.3%¡£ÂËÒº450.7g£¬ÂËÒº»ØÊÕTHFºóÁóµ×ÓÃÓÚÎö¾§Ì×Óá£


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liuqifa: ½ð±Ò+10, ¡ïÓаïÖú 2015-02-28 11:44:12
ÖØ½á¾§£º½«227.3gÎö¾§Â˱ý¼ÓÈëµ½2L¸ÉÔïµÄËÄ¿ÚÉÕÆ¿ÖУ¬¼ÓÈë454.6gTHF£¬ÉýÎÂÖÁ60-65¡æ£¬Ê¹¹ÌÌåÍêÈ«Èܽ⣬±£ÎÂ10min£¬ºó½µÎÂÖÁ50¡æÓý¾§1h£¬½µÎÂÖÁ-15~ -10¡æ±£ÎÂ1h£¬¹ýÂ˵ÃÂ˱ý219.12g£¬HPLC´¿¶È99.3%¡£ÂËÒº450.7g£¬ÂËÒº»ØÊÕTHFºóÁóµ×ÓÃÓÚÎö¾§Ì×Óá£

Recrystalization: Add 227.3 g of filtration cake to a 2L dry flask with 4 necks to which 454.6g THF was then charged, temperature was then raised to 60-65¡æ to completely dissolve the solid. The temperature was kept at that range for 10 min, then lowered to 50¡æ for 1hr to start crystalization, after which, the temperature was lowered to -15~-10 ¡æ for 1 hr. After filtration, 219.12g cake was obtained, the purity was 99.3% as measured by HPLC. Also obtained was 450.7g filtrate, which after the recovery of THF,  can be used as seeds for future crystalization process.
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