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7th August 2012 @ 06:18
Testing standard reaction conditions (25 °C over 1 hour) with a catalyst loading of 0.1 mol%

MNR41-4%20scheme.png
mnr41-12%20table.PNG

To a solution of MNR42-1 (0.2 g, 0.64 mmol) in dry acetonitrile (20 mL, HPLC grade stored over 3 Å molecular sieves for 24 hours) and 3 Å molecular sieves (3 g, dried in microwave) under argon at 0 °C, was added was added acetyl chloride (0.08 mL, 1.15 mmol), 2,6-lutidine (0.10 mL, 0.89 mmol, stored over 3 Å molecular sieves) and PZQ (0.02 g, 0.06 mmol). Yb(OTf)3 solution (0.128 g, in THF (15 mL)) (46 uL, 0.0004 g, 0.0006 mmol) was added and the reaction was stirred at 25 °C for 1 hour.

After 1 hour a sample was taken for mini workup and LCMS. The reaction was left to stir.

Another sample was taken after 2 hours as I was still waiting on LCMS result.

LCMS

mnr41-12_1hour.pdf


Product peak was 93% of the it and standard PZQ therefore referring to >95% conversion within the first hour of reaction.

mnr41-12_2hours.pdf


After 2 hours, the Product peak was 95% of the it and standard PZQ therefore referring to slightly more reaction had taken place in the second hour of the reaction.

Reaction not fully worked up or taken further, happy with this result.
Attached Files
mnr41-12 table.PNG
mnr41-12_1hour.pdf
mnr41-12_2hours.pdf