High there again!
swib dissolved his "product" in boiling MeOH, and let it cool down - only very few crystals appeared - so swim decided to add some Et2O to decrease solubility of the HCl-Salt in the mixture - after one night in the freezer swim filtered the whole thing and got ~1g of product (awful yield!!) - FTIR-analysis will be done soon, to see if any nitrile compund is left... i´ll keep you up to date
Now swim wants to give the PCP-M a second chance - he´d like to use a route without any cyanide dangers (i don´t wanna work with KCN again, without an VERY effective fume hood!! - please, dont do it the way i did!
)
- so there is one method available that looks very nice:
https://www.thevespiary.org/rhodium/Rhodium/chemistry/pcp/bzp_synth.html
I think this method could also be applied to N-Benzoylmorpholine...
1. Let Morpholine and Benzoylchloride react under basic conditions, extract with toluene and distill under aspirator vacuum to yield N-Benzoylmorpholine (the procedure can be found @
www.orgsyn org - search fpr "benzoylpiperidine")
2. React the Benzoylmorpholine with 1,5-Dibromopentane as Mg-Grignard to yield PCPm - (
https://www.thevespiary.org/rhodium/Rhodium/chemistry/pcp/bzp_synth.html
)
Now some specific questions concerning step 2:
1. In the article is described to distill off the Et2O until the reaction mixture reaches 83°C. - the mixture is then hold at this temperature for 16 hours.
- why distill off the solvent?
to increase reactivity? would it also work without distilling off the ether and keeping the mixture @ reflux for about 30 hours?
- may there be some danger of peroxide explosion (ether is from unopened bottle, about 6 months old) when distilling ooff the Et2O? - i think tehre shouldnt be to much danger, because there should be some liquid residue in the flask....
- is there any chance to find the boiling point of N-Benzoylmorpholine and the PCPm-freebase - please help here when possible?
-anyone tried this synthesis?
Many thanks!! I´ll make some photos on the synthesis and write an exclusive report
many thanks bees,
xicori