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14th September 2012 @ 07:21
Mnr: 41-50
Aim repeat of the previous reaction but switching the temperatures.

MNR46-11, 10 mol% Yb at reflux
MNR46-11, stoichiometric Yb at room temperature

MNR46-1%20scheme.png
mnr46-11%20table.PNG

Hazard Assessment
HIRAC MNR41_47_48.pdf


Procedure
To a solution of KAB22-1 (1eq) in HPLC grade acetonitrile (0.03 M) under argon at 0 °C , was added was added acetyl chloride (1.8 eqs), lutidine (1.4 eqs) and Yb(OTf)3 (0.1-1 eqs). The reaction was then stirred at room temperature or at reflux and aliquots taken at noted time intervals for LC analysis.

Sample were taken up to 5 hours then the reaction were left overnight.

As shown in MNR46-10, both reactions showed decrease in product over time.

mnr46-11_plot.PNG

SANY0300.JPG


All reactions quenched on Friday afternoon and TLC only showed traces in 9 and 11. No product visible in reactions containing 100mol%
Attached Files
mnr46-11 table.PNG
mnr46-11_plot.PNG
SANY0300.JPG