Spent all day carefully distilling about a liter of dichloromethane out of a flask containing a solution of something I've been working at very hard indeed. Hopefully now will be when I finally get to produce my desired oxime from the compound in question and break out the sodium metal and isopropanol, and use Na in iPA to reduce the ketoxime to the amine.
The DCM solution has been being stripped at just above its BP (39.6 'C) by keeping it on a warm water steam bath at no more than 60 'C, whilst the compound in DCM solution boils at a far, far far higher boiling point and as such just gets left behind. It will need careful vacuum distillation though, hopefully should come over at about 110-120 'C under a -30mm Hg vacuum, somewhere like that anyway, as currently it is of a light golden amber color, and I want it to be colorless, water clear, before I go to make my oxime. So left the heating on, preset to about 50-60'C (at atmospheric pressure it wouldn't come over until maybe a bit less than 150 'C so no danger of losing it as I slept. Condensing the DCM in a receiver flask so I can redistill it a couple of times and purify it for reuse rather than evaporate it away, since there is so much, just under a liter, maybe 750-800ml. That can be cleaned up and recycled. Once I have my desired ketoxime, I may spend the additional time distilling ethylene glycol antifreeze with concentrated sulfuric acid to produce some 1,4-dioxane, and use the Nurdrage method for reduction of sodium hydroxide with magnesium dust, all those things I have in plenty. And I only need maybe 15g of sodium metal, whilst I have some, its as a hermetically sealed package inside another hermetically sealed package, and its a big ol' 100g block of the stuff (Na metal is one of the lightest of all metals, and 100g is quite a large chunk). I'll store the rest in motor oil after first boiling the oil with dessicant, then filtering it and pouring it into a jar with the screw threads lined in teflon tape, purge the oil with dry argon gas, fill the jar headspace with more argon, which is totally inert to sodium and keep the remaining Na in there. But for this I'd rather make my own. Would, once the dioxane were to be made, give me the excuse I need (I.e having the 1,4-dioxane to hand) to make me a few hundred grams of potassium metal as well, just for the fun of it and because I haven't a jar full of K metal on the lab shelves/cupboards/drawers and there should be one. Why?
No no my dear, the question is not 'why' but 'why not'
