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焕然烟雨

铁虫 (小有名气)

[求助] 如何除去催化剂DBU

求助高手DBU既溶于水也溶于二氯甲烷,而我合成的物质是油溶性的,溶于二氯甲烷,如何从混合体系中除去DBU?如果用萃取应该用什么物质萃取呢?
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R2BBr

木虫 (知名作家)


【答案】应助回帖

★ ★ ★ ★ ★
hsd3521: 应助指数+1, 感谢应助,如不是台湾朋友,烦请用简体中文,谢谢 2012-09-11 19:04:55
hsd3521: 回帖置顶 2012-09-11 19:04:57
焕然烟雨: 金币+5, ★★★很有帮助 2012-09-14 09:23:01
???????:
3?: Originally posted by ??????? at 2012-09-10 16:22:22
??????????????????????????DCM??????????10%HCl?????????????NaCl???????????????????????????DBU??...

A. ????p????? -- ???c???????? DBU ?????????a???????.
B. ???????, ????????? (e.g. 60 ml * 1 ????? DBU Ч????? 20ml *3)
1. Cpd/DBU/solvent + acid ----> 95%DBU/Acid + Cpd/5%DBU/solvent
2. Cpd/5%DBU/solvent + acid ----> 4.75%DBU/Acid + Cpd/0.25%DBU/solvent
?B?m??????????, ?ЙC?? DBU ???N???????? 1%
3. Cpd/0.25%DBU/solvent + acid ----> 0.25%DBU/Acid + Cpd/solvent
?B?m??????????, ?ЙC?? DBU ???N???????? 100 ppm

C. ? back wash (???) ?a???????????. ??????H?? DBU, ????????????????.
4. combined DBU/Acid + solvent ----> 99%DBU/Acid + Cpd/solvent  (back wash)
?????????????O???????????,???3. ?ЙC???c1, 2 ?ЙC????? (?@???? back wash)
4楼2012-09-11 01:54:58
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R2BBr

木虫 (知名作家)


【答案】应助回帖

感谢参与,应助指数 +1
酸水洗去 DBU,  DCM 萃取合成的產物.
2楼2012-09-10 12:29:14
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焕然烟雨

铁虫 (小有名气)

引用回帖:
2楼: Originally posted by R2BBr at 2012-09-10 12:29:14
酸水洗去 DBU,  DCM 萃取合成的產物.

这个先后顺序有要求吗?我之前是先用DCM萃取,然后用10%HCl水溶液萃取,再用NaCl饱和溶液洗再水洗,可是还是有少量DBU的
3楼2012-09-10 16:22:22
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R2BBr

木虫 (知名作家)


???????:
4?: Originally posted by R2BBr at 2012-09-11 01:54:58
A. ????p????? -- ???c???????? DBU ?????????a???????.
B. ???????, ????????? (e.g. 60 ml * 1 ????? DBU Ч????? 20ml *3)
1. Cpd/DBU/solvent + acid ----> 95%DBU/Acid + Cpd/5%DBU/solvent
...

?????????w??????_, ?????. (???????b?P?, ????????? Windows. ???????????????. )
5楼2012-09-12 08:37:14
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xdz1978

至尊木虫 (文坛精英)

持之以恒!

【答案】应助回帖

感谢参与,应助指数 +1
酸水洗就可以了,要百分百去掉是不可能的,总会有点残留
一身正气,两袖清风,三餐温饱,四大皆空!
6楼2012-09-12 10:56:48
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