I am using POCl3 solvent for the reaction, I want to know how to work up or which type of work up method will be suitable for this reaction.
Explanation: On addition of water to POCl3 reaction mixture resulting highly exothermic reaction.
Request: Please suggest some other suitable method or procedure or paper.
If you are using POCl3 as a solvent that indicates that your reaction is sensitive to moisture and you are carrying out the reaction under inert atmosphere.
First of all, you should tell what reaction you are doing and what product you want to isolate, then some one can give you suggestion. Instead, if you ask something like this, others will be wasting their time in giving you a suggestion.
On this platform please ask a question with proper background to your problem, so that appropriate suggestion may come.
Best wishes
Respected sir,
All the detail has been sent to you through email.
please suggest some suitable method.
Dear all, better to focus on getting the reaction product than on how to eliminate the solvent. Extraction may be the easiest way to do that. My Regards
Respected Abdelkader BOUAZIZ sir,
thank you for your suggestion. We are focusing on product "On addition of water to POCl3 reaction mixture resulting highly exothermic reaction." question is how to work up ? how to separate reaction mixture from POCl3 ?
Dear Sunil Kumar, basing on information given, all I can suggest are general tips. Did you tried extraction ? In addition to that column chromatography may be anothor solution. Also (1) note AlCl3 + POCl3 form a complex that is easily and separated, and (2) you can use alcohols to react with POCl3 instead of water. My Regards
Hi;
It is a very sensitive compound to hydrolysis; it reacts violently with humidity and water leading to the formation of phosphoric acid and hydrochloric acid. It decomposes under the action of heat, releasing highly toxic fumes of chlorides and phosphorus oxides.
My best regards
Thank you so much for your response on my query on POCL3. I was looking for this solution. Now my query has been resolved.
Dear Sunil Kumar thank you for your interesting technical question. It depends on the amount of POCl3 you are using. If it's not too much, you can hydrolyze it with ice in the fume hood and neutralize the mixture with NaOH.
For more potentially useful answers about this topic please also have a look at the following closely related discussion:
How can I properly quench POCl3?
https://www.researchgate.net/post/How_can_I_properly_quench_POCl3
Respected Frank T. Edelmann sir,
Thank you for this information, I found it very useful in my current study.
First you should remove excess pocl3 by vaccum distillation then strip RM twice or thrice with DCM ,then add aqueous solution of soda ash or potash (K2Co3). if excess pocl3 is eliminated already , very mild exotherm along with effervescence of CO2 will be observed ,you get product ,the bi -products trisodium phosphate or tripotassium phosphate + Nacl or KCl will remains soluble in excess water.
Check http://orgsyn.org/Content/pdfs/procedures/v89p0380.pdf
Also check https://rtong.people.ust.hk/Organic%20Reaction%20Workup.pdf
And https://www.masterorganicchemistry.com/reaction-guide/elimination-of-alcohols-to-give-alkenes-using-pocl3/
Kindly look at this paper.
Article Phosphorus oxychloride as an efficient coupling reagent for ...
Dear Sunil Kumar thank you again for your interesting technical question. The article suggested by Kiprotich Kiptum is potentially useful, but is is not freely available as public full text. However, the Supplementary Information for this article can be freely downloaded as pdf file. There you can find the work-up procedure for reactions involving POCl3. Basically the reactions are carried out in dichloromethane as solvent. After completion of the reaction, the organic phase is washed sequentially with ice-cooled water, 10% aqueous HCl, saturated aqueous NaHCO3 solution (10 mL), and brine and is then dried over anhydrous sodium sulfate. During the washing procedure the excess POCl3 is hydrolyzed and removed.
Phosphorus Oxychloride as an Efficient Coupling Reagent for the Synthesis of Ester, Amide and Peptide under Mild Conditions
http://www.rsc.org/suppdata/ra/c3/c3ra42887g/c3ra42887g1.pdf
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