| 查看: 318 | 回复: 2 | |||
| 当前主题已经存档。 | |||
吴桂叶金虫 (正式写手)
|
[交流]
【求助】环糊精与羧基反应
|
||
|
想和大家交流请教一下环糊精和酸反应的条件， 比如环糊精与罗丹明反应。反应条件如下： Lissamine rhodamine B ethylenediamine (2 mg, 3.3 mmol) and highmolecular mass CDP (Mw ) 97 kDa, 37.8 mg) were dried under vacuum for 4 h. Dimethyl sulfoxide (DMSO, 3.7 mL) was added to the mixture, followed by 1-ethyl-3-[3-(dimethylamino) propyl]carbodiimide hydrochloride (EDC, 2.6 mg, 13.6 mmol) and N-hydroxysuccinimide (NHS, 1.6 mg,13.6 mmol). The mixture was stirred for 24 h and dialyzed against water using a [color=]MWCO of 25 000 for 72 h in the dark.The polymer-dye conjugate (HRhod) was obtained in 80% yield (32 mg) after lyophilization. The weight percent of rhodamine on the conjugate was determined by measuring the absorbance from rhodamine at 560 nm. 对其中的MWCO of 25 000 透析不太明白。 环糊精与水杨酸反应：SA (0.1036 g, 0.75 mmol) and CDI (0.179 g) were dissolved in 3 ml of DMSO, and the mixture was stirred at room temperature for 30 min. After adding γ-CyD (0.6485 g,0.5 mmol) and TEA (4 ml), the mixture was stirred at room temperature for 18 h. Approximately, 200 ml of acetone was added to the reaction solution, and the precipitate was collected under reduced pressure. The precipitate was purified by ion-exchange column chromatography (DiaionTM HP-20, Mitsubishi Chemical, Tokyo, Japan) and the resulting conjugate was eluted with methanol/water with increasing methanol content. The eluents were monitored by thin layer chromatography (TLC), and the conjugate appeared in the eluents of 30—50% methanol in water. After methanol was removed under reduced pressure, the solution was lyophilized to yield 0.34 g (24%) of SA/γ-CyD conjugate. Rf value_0.75 (TLC: silica gel 60F254 (Merck, Darmstadt, Germany); ethyl acetate–2-propanol–ammonium hydroxide–water (7 : 7 : 5 : 4, v/v); indicator p-anisaldehyde; 其中处理用离子交换柱不太明白，一定要用离子交换柱吗？ [ Last edited by 吴桂叶 on 2009-8-1 at 10:29 ] |
回复此楼» 猜你喜欢
Sci. Bull. 悲剧经验
已经有6人回复
-
提交了我也来说说感想
已经有5人回复
-
今年审到国自然15份，谈谈感受
已经有20人回复
-
国自然评分
已经有4人回复
-
面上本子正文33页，违规吗？会被低分嘛？
已经有11人回复
-
评审有感
已经有22人回复
-
反应很差，大量原料没有反应
已经有6人回复
-
如果工作了想读博，可以边工作边读全日制嘛？
已经有5人回复
-
如何实现卤原子转化
已经有8人回复
-
河北省自然科学基金
已经有3人回复
Bobbie5598
银虫 (正式写手)
- 应助: 0 (幼儿园)
- 金币: 1365.7
- 散金: 10
- 红花: 1
- 帖子: 317
- 在线: 47.8小时
- 虫号: 705214
- 注册: 2009-02-20
- 性别: MM
- 专业: 金属有机化学
2楼2009-08-01 10:36:46
吴桂叶
金虫 (正式写手)
- 应助: 3 (幼儿园)
- 金币: 1121.4
- 散金: 123
- 红花: 1
- 帖子: 447
- 在线: 95小时
- 虫号: 452643
- 注册: 2007-11-05
- 性别: MM
- 专业: 有机合成
3楼2009-08-01 10:42:41
30