Ximik & Cold
Cold
So you’re working on that new compound, right? Tell me the steps and we’ll cut out every redundant move—no waste, no bureaucracy.
Ximik
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.
Cold
Drying under vacuum is fine, but 80 °C is a lot—check if that damages any sensitive groups. 0.01 g catalyst for 0.5 g substrate is 2 % loading; too high? Might drive side reactions. 0.6 g oxidant is 1.2 equivalents—reasonable but keep an eye on stoichiometry. Holding at 50 °C while adding the oxidant is okay; make sure the temperature doesn’t spike. TLC every 15 min is good, but confirm the Rf value matches the expected product. Precipitation in cold hexane should work; ensure the mixture is stirred enough. Filtration under reduced pressure is standard, but if the solid clogs, a short wash with cold hexane can help. Drying at 50 °C for 2 h is fine; just confirm no solvent evaporation losses. Recrystallization from 7:3 ethanol/hexane is a solid choice for most organic products; check that the solvent ratio gives a sharp melting point. Finally, NMR and HRMS will confirm purity—skip them and you’ll get impurities you can’t catch later. No unnecessary steps, but keep a buffer for any unexpected side product.