Up-scaling microscale cyclohexanone synth

[Jubrail]

Any special considerations in upscaling this other than, of course, bigger glassware and multiplying the number of moles used as desired?

Thanks to Rhodium's site, which contains thorough cyclohexanone synth/acquisition info.

Safety: basic, including goggles, lab coat, rubber cleaning-lady gloves on top of latex  and construction worker's dust mask; "bilge-fan" ventilation in well-ventilated room.

Solution of chromic acid prepared by dissolving 8g K dichromate into 40mL H20 in 125mL Erlenmeyer via Buchner.  7mL conc. sulfuric acid added in drops from pipette with gentle swirling between each addition and placed in ice-water bath.  7g lab-grade cyclohexanol dissolved in 25mL H20 in wine decanter with lip for pouing.  Cyclohexanol solution poured into chromic acid solution and mixed in well with stirring rod.  Thermometer left in solution; exothermic oxidation reaction created a rise in temperature not past 140 degrees F.  Flask allowed to cool for 70 min. with occassional swirling while Turkish coffee was prepared with cardamom and drank.  Whole mixture transferred to round-bottom (250mL) containing 35mL water.  Flask set into fractional distillation set-up with stainless steel wool packing.

Mixture distilled resulting in what looked to be under 100mL of distillate, layered into liquid layer and realtively viscous layer.  Transferred to upside-down 1 L plastic bottle with "pop-top."  7g of table salt added and swirled for 5 min.  Pop top opened to separate layers.  Liquid layer extracted with 15 mL diethyl ether and bilge fan employed.  Combined with organic layer and dried with Na2SO4.

Filtered through doubled-up coffee filters through Buchner x2 into round-bottom (250mL, smaller would have been better) and equipped for simple distillation sans condenser.  Flask and stillhead wrapped in two layers of aluminum foil for insulation.  Collection flask resting in the ice-water bath heated on borrowed hot-plate and distillate flask heated in mineral oil bath.  Ether distilled off and cyclohexanone collected at approx. 308 degrees F.  Looks like water.

[Rhodium]

You always need to be careful when scaling up exothermic reactions, do it in steps (not more than 5 x scaleup at a time), carefully monitoring the temperature, and adding the reactants slowly.

Could you please link the synth at my site which you are referring to, as well as report your results of each scale-uplevel you do?

[Aurelius]

Don't go scaling up metal oxidation reactions like that!  Too much waste afterwards (unless you plan on recycling).  try a more green-chem approach like oxidation with hydrogen peroxide or oxone.  maybe a peracid oxidation.

[Jubrail]

I didn't actually do the synth as described, but used it for guidance after comparing molecular structures.  I had a decent yield though, so I think my procedure is a safe bet and has the same general idea as a synth on rhodium's site at:

https://www.thevespiary.org/rhodium/Rhodium/chemistry/pcp/precurs_synth.html

Thanks for the help.