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15th December 2011 @ 23:12
Attempts to sort out the problems of the [url=http://www.organic-chemistry.org/namedreactions/newman-kwart-rearrangement.shtm]Newman-Kwart Rearrangement[/url] using a microwave assisted procedure [b]Hazard and Risk Assessment:[/b] As for [url=http://www.ourexperiment.org/data/files/1537/HIRAC%20MNR17.pdf]HIRAC-MNR17[/url] [b]Procedure MNR20-9[/b] [url=http://www.ourexperiment.org/racemic_pzq/2588/Preparation_of_racOO11binaphthyl22diyl_bisdimethylcarbamothioate_MNR191.html]MNR19-1[/url] (75 mg, 0.16 mmol) was placed in a microwave tube, sealed and heated with 300 W at 200 °C for 20 minutes. Reaction could not get to temperature and starting material did not react. Not enough in the tube to absorb the microwaves? Need to scale up production of starting material. [i]Lab book page complete, MNR[/i] [b]4/01/12 Procedure MNR20-10[/b] A combination of [url=http://www.ourexperiment.org/racemic_pzq/2588/Preparation_of_racOO11binaphthyl22diyl_bisdimethylcarbamothioate_MNR191.html]MNR19-1[/url], [url=http://www.ourexperiment.org/racemic_pzq/3124/Attempts_to_improve_the_preparation_of_racOO11binaphthyl22diyl_bisdimethylcarbamothioate_MNR19.html]MNR19-2 and MNR19-3[/url] (1.140 g, 2.47 mmol) was placed in a microwave tube, sealed and heated with 300 W at 200 °C for 20 minutes. Again, the reaction could not get to temperature and starting material did not react. There was plenty in the tube this time. Need to look into other routes for carrying out this step, ie solvent based approach. 1H NMR MNR20-10 99 % starting material recovered (1.134 g) [i]Lab book page complete, MNR[/i]
Attached Files
MNR20-20 scheme.png
mnr20-10.zip
mnr20-10.pdf