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24432492Acid-mediated Pictet-Spengler of MW29 to give rac-PZQ MNR13-1
Experiments
www.google.com-accounts-o8-id-id=AItOawmHgL4uOJCXiVgu09ud3WRBjgfQtBatmNEMurray Robertson [b]Hazard and Risk Assessment:[/b] As for [url=http://www.ourexperiment.org/racemic_pzq/2422/Acidmediated_PictetSpengler_of_MNR82_to_give_dimethoxyNbenzoylderivative_of_PZQ_MNR122.html]MNR12-2[/url] [b]Procedure[/b] MW29/MW36 (85 mg, 0.25 mmol) was stirred with methanesulfonic acid (1.6 mL, 25 mmol) at room temperature and after 1 hour (first TLC) all the starting material had been consumed. The reaction was quenched with saturated sodium carbonate and extracted with EtOAc (20 mL x2). The organic fractions were dried over magnesium sulfate, filtered and concentrated under reduced pressure. Crude - 76 mg as a yellow oil that showed signs of slowly crystallizing after 24 hours Crude 1H NMR did not match with MNR9-1 - peaks missing 4-6 ppm [data]1466[/data]]]>




Hazard and Risk Assessment:
As for MNR12-2

Procedure
MW29/MW36 (85 mg, 0.25 mmol) was stirred with methanesulfonic acid (1.6 mL, 25 mmol) at room temperature and after 1 hour (first TLC) all the starting material had been consumed. The reaction was quenched with saturated sodium carbonate and extracted with EtOAc (20 mL x2). The organic fractions were dried over magnesium sulfate, filtered and concentrated under reduced pressure.

Crude - 76 mg as a yellow oil that showed signs of slowly crystallizing after 24 hours

Crude 1H NMR did not match with MNR9-1 - peaks missing 4-6 ppm
mnr13-1.pdf
Linked Posts
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24436943Acid-mediated Pictet-Spengler of MW29 to give rac-PZQ MNR13-1
Experiments
www.google.com-accounts-o8-id-id=AItOawmHgL4uOJCXiVgu09ud3WRBjgfQtBatmNEMurray Robertson [b]Hazard and Risk Assessment:[/b] As for [url=http://www.ourexperiment.org/racemic_pzq/2422/Acidmediated_PictetSpengler_of_MNR82_to_give_dimethoxyNbenzoylderivative_of_PZQ_MNR122.html]MNR12-2[/url] [b]Procedure[/b] MW29/MW36 (85 mg, 0.25 mmol) was stirred with methanesulfonic acid (1.6 mL, 25 mmol) at room temperature and after 1 hour (first TLC) all the starting material had been consumed. The reaction was quenched with saturated sodium carbonate and extracted with EtOAc (20 mL x2). The organic fractions were dried over magnesium sulfate, filtered and concentrated under reduced pressure. Crude - 76 mg as a yellow oil that showed signs of slowly crystallizing after 24 hours Crude 1H NMR did not match with MNR9-1 - peaks missing 4-6 ppm [data]1466[/data]]]>




Hazard and Risk Assessment:
As for MNR12-2

Procedure
MW29/MW36 (85 mg, 0.25 mmol) was stirred with methanesulfonic acid (1.6 mL, 25 mmol) at room temperature and after 1 hour (first TLC) all the starting material had been consumed. The reaction was quenched with saturated sodium carbonate and extracted with EtOAc (20 mL x2). The organic fractions were dried over magnesium sulfate, filtered and concentrated under reduced pressure.

Crude - 76 mg as a yellow oil that showed signs of slowly crystallizing after 24 hours

Crude 1H NMR did not match with MNR9-1 - peaks missing 4-6 ppm
mnr13-1.pdf
Linked Entries
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