The Vespiary

The Hive => Newbee Forum => Topic started by: mtnfrogger198 on March 27, 2003, 02:40:00 AM

Title: Glycol Storage ?
Post by: mtnfrogger198 on March 27, 2003, 02:40:00 AM

Is it ok for swim to store the isosafrole monoformyl glycol / formic acid solution, or will it rearrange itself?

Title: Glycol stability
Post by: Rhodium on March 27, 2003, 02:50:00 AM

Post 207172 (missing)

(Ritter: "stability of isosafrole glycol", Methods Discourse)

It will not keep in acid solution though, remove all traces of acid (wash with Na2CO3, water & brine) and it will keep very long.

Title: Sweet, like honey...
Post by: mtnfrogger198 on March 27, 2003, 04:29:00 AM

Thanks Rhodium!

I read the forum containing arguments about the improved performic reaction. I'm still a little unclear on how to undertake the initial extraction. Let me outline...

1) Flood the reaction contents with water
2) Extract with DCM x3
3) Now, is this where we wash with bicarb? <-------
4) Remove the DCM via vac.distillation...
5) Perform the H2SO4 hydrolization

I couldn't find any posts on neutralizing the leftover formic acid with baking soda. Has this been tried, or will it fuck up the glycol?

Thanks again........... ;)

Title: Peracetic
Post by: wolfx on March 27, 2003, 06:28:00 PM

Would the same apply to the peracetic ? I think so, but I would like to have a confirmation.

Also, after the main reaction, there are two NaOH washes ( before the MeOH / H2SO4 reflux ), what else would be necessary before storing the glycol.

Title: Read Labtop extensive write up
Post by: abacus on March 27, 2003, 11:58:00 PM

Look ay Labtops sticky threads, the details you seek are very well described, or UTSE, its all here

If you want to make glycol then as rhodium mentioned remove traces of acid for storage,

But if the goal is to make ketone, then after stirring for 24 hours, pour into a seperating funnel and let the layers seperate.  Remove the DCM layer and distill DCM away until monoformyl glycol is left.  This is done at atmopsheric pressure and until the liquid temperature reaches 80DegC.

Then hydrolyse with 15% H2SO4 as described.  The wash of the crude ketone is NOT done by using NaOH but by using a saturated bicarb solution.  Then vacuum distill the ketone. 

Abacus