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30563194Microwave assisited preparation of (rac)-S,S'-1,1'-binaphthyl-2,2'-diyl bis(dimethylcarbamothioate) MNR20 from MNR19-1
Experiments
plus.google.com-113014781212630252105Murray Robertson [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]]]>Newman-Kwart Rearrangement using a microwave assisted procedure



Hazard and Risk Assessment:
As for HIRAC-MNR17

Procedure
MNR20-9

MNR19-1 (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.

Lab book page complete, MNR

4/01/12

Procedure
MNR20-10

A combination of MNR19-1, MNR19-2 and MNR19-3 (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)

Lab book page complete, MNR
Linked Posts
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]]>2011-12-15T23:12:12+00:002012-01-05T03:11:39+00:006cd9240e5210066af1971b820a86d4ff8https://www.ourexperiment.org/data/2011.xmlhttps://www.ourexperiment.org/data/2017.xmlhttps://www.ourexperiment.org/data/2019.xmlhttp://www.ourexperiment.org/uri/1a9https://www.ourexperiment.org/racemic_pzq/3056/Microwave_assisited_preparation_of_racSS11binaphthyl22diyl_bisdimethylcarbamothioate_MNR20_from_MNR191.htmlhttps://www.ourexperiment.org/racemic_pzq/3056/Microwave_assisited_preparation_of_racSS11binaphthyl22diyl_bisdimethylcarbamothioate_MNR20_from_MNR191.htmlhttps://www.ourexperiment.org/racemic_pzq/3056/Microwave_assisited_preparation_of_racSS11binaphthyl22diyl_bisdimethylcarbamothioate_MNR20_from_MNR191.xmlhttps://www.ourexperiment.org/racemic_pzq/3056/Microwave_assisited_preparation_of_racSS11binaphthyl22diyl_bisdimethylcarbamothioate_MNR20_from_MNR191.pnghttps://www.ourexperiment.org/racemic_pzq/3056/Microwave_assisited_preparation_of_racSS11binaphthyl22diyl_bisdimethylcarbamothioate_MNR20_from_MNR191.xml?revision=3056https://www.ourexperiment.org/racemic_pzq/3056/Microwave_assisited_preparation_of_racSS11binaphthyl22diyl_bisdimethylcarbamothioate_MNR20_from_MNR191.xml?revision=3057https://www.ourexperiment.org/racemic_pzq/3056/Microwave_assisited_preparation_of_racSS11binaphthyl22diyl_bisdimethylcarbamothioate_MNR20_from_MNR191.xml?revision=3058https://www.ourexperiment.org/racemic_pzq/3056/Microwave_assisited_preparation_of_racSS11binaphthyl22diyl_bisdimethylcarbamothioate_MNR20_from_MNR191.xml?revision=3059https://www.ourexperiment.org/racemic_pzq/3056/Microwave_assisited_preparation_of_racSS11binaphthyl22diyl_bisdimethylcarbamothioate_MNR20_from_MNR191.xml?revision=3160https://www.ourexperiment.org/racemic_pzq/3056/Microwave_assisited_preparation_of_racSS11binaphthyl22diyl_bisdimethylcarbamothioate_MNR20_from_MNR191.xml?revision=3161https://www.ourexperiment.org/racemic_pzq/3056/Microwave_assisited_preparation_of_racSS11binaphthyl22diyl_bisdimethylcarbamothioate_MNR20_from_MNR191.xml?revision=3162https://www.ourexperiment.org/racemic_pzq/3056/Microwave_assisited_preparation_of_racSS11binaphthyl22diyl_bisdimethylcarbamothioate_MNR20_from_MNR191.xml?revision=3174https://www.ourexperiment.org/racemic_pzq/3056/Microwave_assisited_preparation_of_racSS11binaphthyl22diyl_bisdimethylcarbamothioate_MNR20_from_MNR191.xml?revision=3175https://www.ourexperiment.org/racemic_pzq/3056/Microwave_assisited_preparation_of_racSS11binaphthyl22diyl_bisdimethylcarbamothioate_MNR20_from_MNR191.xml?revision=3176https://www.ourexperiment.org/racemic_pzq/3056/Microwave_assisited_preparation_of_racSS11binaphthyl22diyl_bisdimethylcarbamothioate_MNR20_from_MNR191.xml?revision=3194https://www.ourexperiment.org/racemic_pzq/3056/Microwave_assisited_preparation_of_racSS11binaphthyl22diyl_bisdimethylcarbamothioate_MNR20_from_MNR191.xml?revision=7318
30567318Microwave assisited preparation of (rac)-S,S'-1,1'-binaphthyl-2,2'-diyl bis(dimethylcarbamothioate) MNR20 from MNR19-1
Experiments
plus.google.com-113014781212630252105Murray Robertson [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]]]>Newman-Kwart Rearrangement using a microwave assisted procedure



Hazard and Risk Assessment:
As for HIRAC-MNR17

Procedure
MNR20-9

MNR19-1 (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.

Lab book page complete, MNR

4/01/12

Procedure
MNR20-10

A combination of MNR19-1, MNR19-2 and MNR19-3 (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)

Lab book page complete, MNR
Linked Entries
This entry is linked by:
]]>2011-12-15T23:12:12+00:002015-08-28T15:20:04+00:006https://www.ourexperiment.org/data/2011.xmlhttps://www.ourexperiment.org/data/2017.xmlhttps://www.ourexperiment.org/data/2019.xmlhttp://www.ourexperiment.org/uri/1a9https://www.ourexperiment.org/racemic_pzq/3056/Microwave_assisited_preparation_of_racSS11binaphthyl22diyl_bisdimethylcarbamothioate_MNR20_from_MNR191.htmlhttps://www.ourexperiment.org/racemic_pzq/3056/Microwave_assisited_preparation_of_racSS11binaphthyl22diyl_bisdimethylcarbamothioate_MNR20_from_MNR191.htmlhttps://www.ourexperiment.org/racemic_pzq/3056/Microwave_assisited_preparation_of_racSS11binaphthyl22diyl_bisdimethylcarbamothioate_MNR20_from_MNR191.xmlhttps://www.ourexperiment.org/racemic_pzq/3056/Microwave_assisited_preparation_of_racSS11binaphthyl22diyl_bisdimethylcarbamothioate_MNR20_from_MNR191.pnghttps://www.ourexperiment.org/racemic_pzq/3056/Microwave_assisited_preparation_of_racSS11binaphthyl22diyl_bisdimethylcarbamothioate_MNR20_from_MNR191.xml?revision=3056https://www.ourexperiment.org/racemic_pzq/3056/Microwave_assisited_preparation_of_racSS11binaphthyl22diyl_bisdimethylcarbamothioate_MNR20_from_MNR191.xml?revision=3057https://www.ourexperiment.org/racemic_pzq/3056/Microwave_assisited_preparation_of_racSS11binaphthyl22diyl_bisdimethylcarbamothioate_MNR20_from_MNR191.xml?revision=3058https://www.ourexperiment.org/racemic_pzq/3056/Microwave_assisited_preparation_of_racSS11binaphthyl22diyl_bisdimethylcarbamothioate_MNR20_from_MNR191.xml?revision=3059https://www.ourexperiment.org/racemic_pzq/3056/Microwave_assisited_preparation_of_racSS11binaphthyl22diyl_bisdimethylcarbamothioate_MNR20_from_MNR191.xml?revision=3160https://www.ourexperiment.org/racemic_pzq/3056/Microwave_assisited_preparation_of_racSS11binaphthyl22diyl_bisdimethylcarbamothioate_MNR20_from_MNR191.xml?revision=3161https://www.ourexperiment.org/racemic_pzq/3056/Microwave_assisited_preparation_of_racSS11binaphthyl22diyl_bisdimethylcarbamothioate_MNR20_from_MNR191.xml?revision=3162https://www.ourexperiment.org/racemic_pzq/3056/Microwave_assisited_preparation_of_racSS11binaphthyl22diyl_bisdimethylcarbamothioate_MNR20_from_MNR191.xml?revision=3174https://www.ourexperiment.org/racemic_pzq/3056/Microwave_assisited_preparation_of_racSS11binaphthyl22diyl_bisdimethylcarbamothioate_MNR20_from_MNR191.xml?revision=3175https://www.ourexperiment.org/racemic_pzq/3056/Microwave_assisited_preparation_of_racSS11binaphthyl22diyl_bisdimethylcarbamothioate_MNR20_from_MNR191.xml?revision=3176https://www.ourexperiment.org/racemic_pzq/3056/Microwave_assisited_preparation_of_racSS11binaphthyl22diyl_bisdimethylcarbamothioate_MNR20_from_MNR191.xml?revision=3194https://www.ourexperiment.org/racemic_pzq/3056/Microwave_assisited_preparation_of_racSS11binaphthyl22diyl_bisdimethylcarbamothioate_MNR20_from_MNR191.xml?revision=7318https://www.ourexperiment.org/racemic_pzq/3056/Microwave_assisited_preparation_of_racSS11binaphthyl22diyl_bisdimethylcarbamothioate_MNR20_from_MNR191.xml?revision=-1