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lijy 发表于 2008-7-2 18:49

氨基酸上Boc

实验内容是手性苯丙胺酸上Boc,拿到的文献是德文的,看不懂,大概是用三乙胺,那位高人进行过这方面的实验,或有这方面的文献,请多多帮助,就实验细节具体指导下,多谢!

tutu2000 发表于 2008-7-2 19:56

回复 1# lijy 的帖子

我一般用无机碱,好处理,比如NaHCO3.

yushouyun 发表于 2008-7-3 03:02

Boc-Phe直接买,很便宜。

如果要自己做的话, To a suspension of Phe in H2O and THF (5:1, Concentration about 0.5 M)at 0  degree were added NaOH (2.0 eq.) and Boc2O (1.2 eq.). The mixture was stirred at rt for several hours (overnight is OK). The resulting mixture was diluted with H2O and washed with ether (remove Boc2O) ,and aqueous phase acidify with HCl (aq.), extracted with EtOAc (3*) and washed with brine. Concentration gave the crude product. It is so pure that you can use it without further purification. Most of time you got viscous oil. If you want to obtain crystal, you can crystallize it with EtOAc and hexanes.

sunyalei508 发表于 2008-10-2 22:12

回复 3# yushouyun 的帖子

二氯甲烷作溶剂,三乙胺作碱。零摄氏度反应3小时即可

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