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31st August 2012 @ 07:23
Mnr: 41-50
Attempts To Cyclise KAB18-1 using AcCl


Hazard Assessment
HIRAC MNR41_47_48.pdf

To a solution of KAB18-1 (1eq) in HPLC grade acetonitrile (0.03 M) under argon at ambient temperature, was added was added acetyl chloride (1.8 eqs), base (1.4 eqs) and catalyst (0.4 eqs). The reaction was then stirred at room temperature (19 °C) over the weekend.

Monday morning

45-2 was a clear yellow solution
45-3 was a cloudy yellow mixture
45-4 was a cloudy yellow mixture

45-2 was spilt while trying to take a TLC, over 75% of it lost.

2 hours

Work Up

MNR45-3 looked the most promising by TLC although the spots were very faint. Column 40% EtOAc/Hex

Frac 15-30 - 15.366g

Frac 32-42
Attached Files
mnr45-2 table.PNG
2 hours