A vacuum distillation, to strip the excess reactants from a synthesis of mine. Set up for distillation, flask containing what is left of the two reactants+a dash of catalyst in a bowl on the hotplate thats full of a mixture of ethylene glycol and water, whilst the other end of the condenser is led into a pan, each with a distillation adapter plugged into the respective flask necks, the rxn still flask with a 3-way adapter plugged in (one end for the RBF, one a thermometer port and the last leading into the condenser which itself is connected to a simple recirculating coolant loop I rigged up from a fish pond pump, and the other end of it ending n a vacuum distillation adapter bend, attached flask sitting in a bath of ice/hydrochloric acid/ethylene glycol to ensure the condensate doesn't escape, after having evacuated it down to a fraction of an atmosphere and clamped it off to maintain the negative pressure without keeping the vac source on constantly so as not to exhaust the condensate from the inside of the flask to the lab atmosphere, because one of the reactants is cheap enough, but the other is rather difficult and 'watched' so is rather precious and often difficult to obtain safely without attracting unwanted attention, so it's being distilled off instead of just chemically separated and discarded, that way I can recycle it instead and reuse the portion thats left over
Distillate seems like its just about beginning to have the first few drops come over, along with some traces of methanol (which is just rubbish in this context), when everything is gone and collected in the receiver flask, hopefully, my compound will be almost ready, just needing washing with some dried glacial acetic acid, ice cold and then with ice cold water.
