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10th August 2012 @ 07:15
Mnr: 41-50
Repeat of MNR41-16 but starting with KAB18-1

MNR45-1%20scheme.png
mnr45-1%20table.PNG

To a solution of KAB18-1 (0.1 g, 0.48 mmol) in HPLC grade acetonitrile (10 mL) and under argon at 0 °C, was added was added acetyl chloride (0.061 mL, 0.86 mmol), 2,6-lutidine (0.077 mL, 0.67 mmol, fresh out of a new bottle). The reaction was then stirred at room temperature (19 °C) for 2.5 hours.

After 2.5 hours a sample was taken for mini workup and LCMS. The reaction was left to shake.

TLC after 2.5 hours showed signs of some reaction but not completion. Reaction left over the weekend due to time constraints.

mnr45-1_TLC_1hour.jpg


LCMS

After 2 hours the LCMS showed what could be traces of product but the MS was very messy in that region and could therefore have resulted in product forming in the MS?

mnr45-1_2hours.pdf


The reaction was left to sit for a couple of days due to other commitments but was eventually worked up to see if any product was present.

The mixture was washed saturated sodium bicarbonate solution (15 mL) and the aqueous layer was extracted with ethyl acetate (3 × 30 mL). The organic fractions were combined, dried over MgSO4, filtered and concentrated under reduced pressure to yield a yellow oil (0.118 g)
Attached Files
MNR45-1 scheme.png
mnr45-1 table.PNG
mnr45-1_TLC_1hour.jpg
mnr45-1_2hours.pdf