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29th August 2012 @ 02:15
Mnr: 41-50
Varying The Reaction Conditions of MNR41. MNR41-17, MNR41-18 and MNR41-19
MNR41-17 - no base, no acid
MNR41-18 - no base, Yb(OTf)3
MNR41-19 - no base, YbCl3

MNR41-4%20scheme.png
mnr41-17_18_19%20table.PNG

Hazard Assessment
HIRAC MNR41_47_48.pdf


Procedure
To a solution of MNR42-1 (1eq) in HPLC grade acetonitrile (0.03 M) under argon at ambient temperature, was added was added acetyl chloride (1.8 eqs) and catalyst (0.4 eqs). The reaction was then stirred at room temperature (19 °C) for 4 hour. (too busy doing other stuff)

Work Up

The mixture was washed saturated sodium bicarbonate solution (10 mL) and the aqueous layer was extracted with ethyl acetate (3 × 15 mL). The organic fractions were combined, dried over MgSO4, filtered and concentrated under reduced pressure to yield a yellow oil.

Crude NMR

mnr41-17_crude.pdf

mnr41-18_crude.pdf

mnr41-19_crude.pdf


All 3 showed signs of product, columns required
Attached Files
HIRAC MNR41_47_48.pdf
mnr41-17_18_19 table.PNG
mnr41-17_crude.pdf
mnr41-18_crude.pdf
mnr41-19_crude.pdf