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16th April 2012 @ 05:14
MNR11-13%20scheme.png

MNR11-13%20table.PNG

Hazard and Risk Assessment:
HIRAC MNR11-13_TfOH.pdf


Procedure:

To a stirring solution of MNR8-3 (3.90 g, 8.4 mmol) in toluene (100 mL) at 0 °C was added TfOH (0.1 mL, 0.84 mmol) under argon, drop-wise. The reaction was then stirred at 0 °C for 90 minutes then allowed to reach room temperature and stirred for a further 1 hour.

The reaction should have been worked up at this time but due to meetings and other stuff it was left overnight at room temperature.

The reaction was neutralised with saturated sodium hydrogen carbonate and the aqueous layer was separated then washed with EtOAc (100 ml x 3). The organic fractions were combined, dried over magnesium sulfate, filtered and concentrated under reduced pressure to give a pale yellow oil.

crude 3.975 g

Column 75-100% EtoAc/Hex

Fracs 20-36 2.046 g, as a white fluffy solid - 65 %

Frac 37-47 0.280 g, orange solid - 9 % - traces of impurities but mainly product.
Attached Files
HIRAC MNR11-13_TfOH.pdf
MNR11-13 scheme.png
MNR11-13 table.PNG