How to run a reaction at 450 °C?
Hello, I am a first year organic PhD student. There is a compound I want to synthesize for my research, but the only reported synthesis of it is at 450 °C for 3 days. The reaction vessel must be sealed to prevent the starting material and product from evaporating away. Boro-silicate is only recommended to operate at 450 °C for 12 hours so I need something other than a rbf or pressure tube. I have a heating mantle that should get up to 450 C and the temperature probe on my hot plate is rated for up to 500 C. I just need a reaction vessel.
The options I have seen are making your own pressure tube with an Inconel tube (Ni/Cr/Fe alloy that is corrosion and oxidation resistant even in harsh conditions) and swagelok fittings, or if you purchase an entire tubular furnace it comes with a metal reaction vessel. I was wondering if there were any stand alone reaction vessels that I could purchase and put on my heating mantle.
If anyone has any experience on how to run a reaction at this temperature without having to own a specialized furnace/autoclave I would love to hear how you did it and what reaction vessel you used.
My research partner really wants me to synthesize this compound so we are going to just try in an old boro-silicate schlenk flask that we won't care if it breaks. We are going to completely evacuate the flask before heating to reduce the pressure that will build while heated. I am also most definelty setting up a blast shield around this reaction.