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29th May 2012 @ 04:32

Hazard and Risk Assessment:

HIRAC MNR37.pdf

Procedure: A mixture of rac-PZQ (1.0 g, 3.2 mmol) and sulfur (0.210 g, 6.4 mmol) under argon was heated at 190°C for 15 minutes by use of a heat gun. The dark brown solid was dissolved in ethyl acetate, evaporated on silica gel and purified by column chromatography (20-40% EtoAC/Hex)

Frac 17-30 - 0.455 g, 1.46 mmol, 46 % as a yellow solid

Frac 40-44 - 0.328 g, 1.05 mmol, 33 % recovered PZQ

1 H NMR 13C NMR

FCC fractions ran in 50% EtOAC/Hexane

mnr37-1 in 50% EtOAc/Hexane

mnr37-1_frac17-30.zip

 

IR 

enediamide IR MNR37-1 dont include.jpg

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1H NMR data from MW59-7 recently found, uploaded here

enediamide NMR MW59-7 dont include.jpg

Scale-up: Oxidation of N-benzoyl-PZQ by sulfur (MW59-7)

Attached Files
HIRAC MNR37.pdf
mnr37-1 table.PNG
MNR37-1 scheme.png
mnr37-1 in 50% EtOAc/Hexane
mnr37-1_frac17-30.zip
mnr37-1_frac17-30.pdf
mnr37-1_frac17-30_13C.pdf
enediamide IR MNR37-1 dont include.jpg
enediamide NMR MW59-7 dont include.jpg