Sciencemadness Discussion Board

high vac distillation of piperidone intermediate

chemrox - 22-7-2014 at 13:52

https://www.sciencemadness.org/whisper/viewthread.php?tid=84...

I'm not exactly following up on this thread as I wanted advice and information on a technical issue related to piperidone synthesis. My vacuum setup is a double chamber vacuum line with a mechanical oil pump and Cartesian manostat along with the manometer. I have several procedures that require me to maintain about 0.3 mm. My equipment remains leaky as indicated by the manostat not settling down. This means I have to control the vacuum manually and that gets tiresome. The vacuum lines are equipped with several, 4 I think, high vac, teflon valves. I think what I need to do is disassemble the whole shebang and clean it very thoroughly. Here's where I'm stuck; I'm afraid of breaking the valves where the nobs attach to the cutoff. I haven't found a manual or writeup on doing the cleaning. I do have a little more of the piperidones than I need