Sure, here’s a stripped‑down version of the protocol for the new compound. 1. Dry all glassware under vacuum and pre‑heat to 80 °C to remove moisture. 2. Charge the flask with the starting material (0.5 g) and dissolve in 20 mL of anhydrous acetone. 3. Add the catalyst (0.01 g) and stir for 5 min to allow full complexation. 4. Slowly pour the oxidant (0.6 g) over the reaction mixture while maintaining 50 °C. 5. Monitor the progress by TLC (hexane/ethyl acetate 3:1) every 15 min; the spot should disappear after ~45 min. 6. Cool to room temperature, then pour the mixture into 50 mL of cold hexane to precipitate the product. 7. Filter under reduced pressure, wash the solid with 10 mL of hexane, and dry at 50 °C for 2 h. 8. Recrystallize from ethanol/hexane (7:3) to obtain the pure compound; expect ~80 % yield. 9. Verify purity by NMR and HRMS. That’s the minimal sequence; any skipped step will compromise yield or purity, so don’t bother shaving off the recrystallization unless you’re willing to tolerate impurities.

Thanks for the feedback, that’s exactly the level of detail I need. I’ll tweak the protocol a bit. 1. Keep the glassware dry, but lower the pre‑heat to 60 °C instead of 80 °C so any heat‑labile groups stay intact. 2. Use 0.008 g of catalyst (1.6 % loading) – that should reduce the chance of over‑catalysis while still driving the reaction. 3. The oxidant stays at 1.2 equivalents (0.6 g), but I’ll add it dropwise over 10 min to keep the temperature from spiking. 4. Hold the reaction at 50 °C, but monitor the bath temperature continuously; if it rises above 55 °C, pause the addition. 5. TLC every 15 min, and I’ll run a quick reference of the product Rf (hexane/ethyl acetate 3:1) before starting to be sure. 6. Stir the mixture gently for 10 min after the oxidant is fully added to ensure a uniform precipitation when I pour it into cold hexane. 7. If filtration clogs, a short wash with 5 mL of cold hexane will loosen the cake and keep the solids from sticking. 8. Dry the solid at 50 °C, but I’ll monitor the mass after 1 h; if it drops, I’ll let it sit longer. 9. Recrystallize from a 7:3 ethanol/hexane mix, but I’ll check the solubility at 10 °C first to get a sharp melt point. 10. Finally, run the NMR and HRMS – skipping that step is a recipe for hidden impurities. That buffer for side products should catch any unexpected by‑products early.

Got it. I’ll pull the catalyst from a certified source and run a quick purity test before loading. I’ll keep the 55 °C ceiling; if it touches 60 °C, I’ll slow the addition further. I’ll do a 10 °C solubility test and take a melting point before and after recrystallization to catch any amorphous material. Mass will be logged after each 30 min interval during drying to spot solvent loss. And I’ll double‑check the Rf reference with a small control spot to avoid mis‑assignment. No extra steps, just tight control.