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9th March 2012 @ 03:22
Testing reactivity of Michael-acceptor of ZYH 6-2 (PMY 41-1) using benzylthiol at 40 °C (close to biological temperatures).


Reaction Start Time: 14.20 09/03/12
ZYH 6-2 (20 mg, 0.05 mmol, 1 equiv.) was stirred in DCM (10 mL). Benzylthiol (27 μL, 0.23 mmol, 5 equiv.) was added and the reaction heated to 40 °C. After 68 hours, solvent had evaporated. A sample of the mixture showed starting materials only by 1H NMR. No peaks consistent with expected product. K2CO3 (approx 0.1 g) was added. After 1 hour, the reaction is a solution with solid base. Stirred at room temperature for approx 20 hours. 1H NMR shows change but no obvious expected product peaks. TLC consistent with SM and some minor products. ESI mass spec. shows only SM. But no mass consistent with benzylthiol adducts.

1H NMR 68 hours

Mass Spec:
ESI mass spec

Risk and Hazard Assessment:
Risk Assessment
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