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16th March 2012 @ 04:02

Resolution of MNR26-1 with (+)-dibenzoyl-D-tartaric acid (MNR5-1)

Hazard and Risk Assessment: As for MNR2-1

MNR26-1 (016 g, 0.61 mmol) and MNR5-1 (0.29 g, 0.61 mmol) was dissolved in a mixture of isopropanol (3 mL) and water (3 mL) and heated till the reagents went into solution. After standing at room temperature overnight no crystals appeared. The reaction mixture was concentrated and taken up in IPA (25 mL) and hexane (15 mL) with heating, allowed to cool to room temperature and left in the freezer overnight. No crystals formed but a small trace of brown solid did. It was filtered off and the solvent was concentrated. The resulting crude was then taken up in IPA (20 mL) and heated to 60 C in a water bath. Hexane (20 mL) was added and the flask was left to stand open at room temperature. After approximately 1 week sitting open in the back of the fume hood crystals started to form, after being left for 3 mores days the crystals were filtered and washed with hexane and EtOAc. More more solid crashed out of this wash and the filtrated was reduced in volume and filtered again, washing with EtOAc.

First crop - fine white solid/crystals 0.055 g Second crop - off white solid 0.055 g

Both crops were kept separate and mixed with water (2 mL) and taken to pH 11 with the addition of NaOH solution (2M) and extracted with DCM (4 ml x 3). The organic fractions were combined, dried over magnesium sulphate, filtered and concentrated under reduced pressure to give...

 

IR 

5f S IR MNR30-1.jpg
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mnr30-1 table.PNG
mnr31-1 table.PNG
MNR30-1 scheme.png
mnr30-1 table.PNG
5f S IR MNR30-1.jpg