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Topic: Column Chromatography  (Read 2519 times)

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Offline ikakurnia

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Column Chromatography
« on: February 03, 2015, 04:57:00 AM »
how to recover my nitro eugenol compound from saturated silica in chromatography column? i was use liquid chromatography.
thank you :)

Offline k1mng

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Re: Column Chromatography
« Reply #1 on: February 03, 2015, 05:29:24 AM »
Hi ikakurnia,

If you were following a prep it should have some information on recovering the compound. Have you tried flushing through the compound with any strongly eluting solvent systems yet?

Offline TheUnassuming

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Re: Column Chromatography
« Reply #2 on: February 03, 2015, 08:07:42 AM »
What solvent system are you using?
When in doubt, avoid the Stille coupling.

Offline ikakurnia

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Re: Column Chromatography
« Reply #3 on: February 03, 2015, 08:41:13 AM »
i have flush with n hexane and DCM, but the silica was saturated, so my compound doesn't good separated. The compound should be dissolve in DCM, but it dissolve to in hexane to. I was wrong when adding slurry of silica. the slurry of silica i use isn't notice the ratio between gram of silica and gram of sample. Sample that containing nitro eugenol was 4.5 g, but i use silica measly, so the silica was going saturated.
« Last Edit: February 03, 2015, 08:56:40 AM by ikakurnia »

Offline ikakurnia

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Re: Column Chromatography
« Reply #4 on: February 03, 2015, 09:15:23 AM »
i use acetonitril as a solvent in sample containing nitro eugneol, but it measly because it has evaporate.

Offline TheUnassuming

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Re: Column Chromatography
« Reply #5 on: February 03, 2015, 12:33:10 PM »
Ok, well your solvent system is still relatively nonpolar so you have a lot of room to play.  Try increasing the polarity of your mobile phase up to 15% MeOH in EtoAc.  It should clean anything off the column without getting appreciable silica contamination off the column. 
Remember that just because something is soluble in a solvent doesn't mean it will come off a column well using just that solvent.  DCM is a great example of this.
When in doubt, avoid the Stille coupling.

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