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Originally posted by hunter0308 at 2010-1-15 21:06:
怎么想起来加水？？？全重排成脲了！！！

[ Last edited by hunter0308 on 2010-1-15 at 21:11 ]

参考文献的哦
To a solution of 1,3-dimethyl-5,6-
diaminouracil (8a, 3.50 mmol) and 1-ethyl-2-[3-(dimethylamino)
propyl]-carbodiimide hydrochloride (EDAC;
5.11 mmol) in 40 mL dioxane/H2O (1:1) was added the
appropriate commercially available carboxylic acid (9,
3.81 mmol). The pH of the suspension was adjusted to 5
with 2 Maqueous hydrochloric acid and stirring was continued
for an additional 2 h. The reaction mixture was
neutralized with 1 M aqueous sodium hydroxide, cooled
to 0 C, and the resulting precipitate was collected by filtration
，

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Originally posted by zph405 at 2010-1-15 19:06:
EDCI缩合剂我经常用，我做的时候都是绝对干燥的，不能有水的，一般情况是，先把EDC和酸混合起来活化2小时，然后在加入胺，溶剂量适当就行，因为现在天冷，你可以适当提高一下温度，30~35°C即可。还有就是，有可能 ...

胺的活性应该可以的啊，我附上了结构

用EDCI 和HOBt

EDC一般和HOBt 连用，再者再加略大于1eq的DIEA

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Originally posted by wz0412052 at 2010-1-15 22:04:

参考文献的哦
To a solution of 1,3-dimethyl-5,6-
diaminouracil (8a, 3.50 mmol) and 1-ethyl-2-[3-(dimethylamino)
propyl]-carbodiimide hydrochloride (EDAC;
5.11 mmol) in 40 mL dioxane/H2O (1:1)  ...

什么杂志上的？？？
看这个综述：
Tetrahedron 61 (2005) 10827–10852
此外：
J. Am. Chem. Soc., 1999, 121 (43), pp 10004–10011
J. Am. Chem. Soc., 2002, 124 (4), pp 520–521
你去看上面两篇的操作去。

EDCI通常要和HOBt合用的，单纯的EDCI反应较慢，反应会产生脲副产物，反应完以后用brine洗两遍，把EDCI和HOBt和酸先搅一下，然后把胺稀释后滴加到上个mixture中，室温搅拌或提高温度，反应会在一两个小时内完成

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Originally posted by wz0412052 at 2010-1-15 22:07:

胺的活性应该可以的啊，我附上了结构

那就是你的pH问题了，溶液肯定不能为酸性的，你可以加点三乙胺，不加也行（几乎中性)

最好用无水溶剂，我们一般EDC都是和HOBT混合使用的(1.5:0.5N)