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16th July 2012 @ 00:49
MNR7-1_scheme.png
MNR7-1%20table.PNG

Hazard and Risk Assessment:
HIRAC MNR7.pdf


Procedure:
rac-PZQ (13.0 g, 41.6 mmol) was dissolved in a mixture of EtOH (80 mL) and 1M HCl (420 mL) and heated to reflux for 14 h. The solution was allowed to cool to room temperature then cooled in an ice bath, basified with NaOH pellet (approx 22 g, pellets used to minimise volume of aqueous material) to pH 12-13 and extracted with DCM (4 x 200 mL). The organic fractions were combined, dried over magnesium sulphate, filtered and concentrated under reduced pressure to give a clear oil which was placed on the high vac for 1 hour by which time the oil had crystallized into white crystals (9.4 g)

Recrystallisation in toluene:hexane (50 mL:5 mL)

After standing in the freezer overnight the crystals were filtered and washed with toluene:hexane (50:50 mL) and dried under vacuum to give off white/pale yellow crystals 7.212 g, 35.66 mmol, 86 %