[rita87]

Hi,
Do you know how I can add an air sensitive solid and a liquid to a schlenk tube equipped with rubber septum using hypodermic syringe? well I know how to transfer the liquid, but the problem is the solid one.
Can I store an air sensitive solid in a sure/seal bottle?if yes how can i transfer it from that bottle?

Thank you

[azmanam]

make a solution of it, transfer it as you would a liquid, remove the solvent under vacuum, back fill the vacuum with inert atmosphere.

[azmanam]

or dissolve it in DCM or ether or something really low boiling and just blow the solvent off with a strong stream of argon or nitrogen (with a good venting needle!)

[rita87]

how would you make a solution of it, as it is air sensitive i am not sure how to get it out of its container.

[azmanam]

what container is it in?  how air sensitive is it?  Can you not flame dry a flask, pop the septum long enough to dump your solid in, then cap the flask again?  Is it that sensitive?  What happens to it?  pyrophoric, hygroscopic, deliquescent?

If it's in a container with a septum already, then just syringe in solvent (with a venting needle and a positive pressure of inert gas).  If it's in a screw-top bottle, then the manufacturers must hate you, or expect you to use it in a glove box.  In which case some inorganic lab probably has a glove box with solvent in it.

My guess is that you'll be able to do the 'dump out really quick' method.  otherwise we'll need more information.

[rita87]

Thank you.
Well, I am not sure how sensitive it is, the compound is Dimethylamino isoborneol. I think adding liq to the container with septum sounds good.
I think Ether should be a good choice?

[azmanam]

Ether's expensive.  If you're just going to vac it back down, I like DCM.

[nj_bartel]

No access to a dry box I assume?

[Squirmy]

the compound is Dimethylamino isoborneol.

based on the Org Syn prep, I'd be surprised if they did all of the workup steps under inert atmosphere or in a dry box. They offer a cautionary note about storage under nitrogen or argon, but they don't say anything about special techniques or glassware used for the filtration. Org Syn gives you details like "500-ml, single-neck round-bottomed flask" that you rarely see in other journals nowadays, so it would be strange not to mention more specialized techniques.

http://www.orgsyn.org/orgsyn/orgsyn/prepContent.asp?prep=v79p0130

My point, it's probably not THAT air-sensitive. If I had a dry box, I'd use it for any transfers. If not, you can probably work quickly with it and flush the atmosphere of the bottle with an inert gas. Or, if you know what your reaction solvent is going to be, you could make a stock solution of a convenient, known concentration to store in your Schlenck tube.

[rita87]

I am following this article  http://www.orgsyn.org/orgsyn/orgsyn/prepContent.asp?prep=V79P0139
According to this DAIB is transferd "through a rubber septum using hypodermic syringes ",so i assume it should be sensitive, other wise why should we use a rubber septum. and apparently i should use a hypodermic syringe to transfer it, so the compound needs to be liq , i think.

[rita87]

Is there any other way for transfering a solid with a hypodermic syringe?

[gfunk]

The paper that that paper references (the one Squirmy referenced) says that compound is an oil?  Even if it were a solid, it says it slowly decomposes in air, so it shouldn't be too much trouble to work with.  It's not like it's pyrophoric or anything!

[macman104]

I was just about to post what gfunk did.  The paper says it is an oil, and that it only slowly decomposes under air.  Not that it is highly pyrophoric or anything.

[rita87]

OMG you ar so right, don't know why i thought that was a solid.Thanks both of you.