Rather pleased with myself, after spending a good few days working in the lab on one particular project, and spending both another full night and almost all the following day slowly distilling off the solvent in which my project was dissolved. Finally, nothing more coming over at just over the boiling point of the solvent, meticulously stripping it away and catching nearly a liter of methylene chloride in the receiving flask (the product is much higher boiling, a couple of hundred 'C at atmospheric pressure and needs to be vacuum distilled in order to avoid decomposition, so when stripping the solvent the product is left behind in the pot whilst the CH2Cl2 comes over into the receiving flask).
Been meticulously distilling, so as to have the solvent come over at a rate of a couple of drops every second to 1.5 seconds or so at no more than 55-60 degrees or so. What I was working on all stayed behind in the pot as desired, and looks fairly good, not quite clear yet, that'll take the distillation at reduced pressure using the venturi pump, but its a light, see-through golden color, like amber but considerably lighter. And after all the time taken to get it after as many as 9-10 steps, including the various purification and workup steps needed to prepare a catalyst I needed for the reaction to produce the intermediate, production of the intermediate via a rather nifty technique involving microwave irradiation, crystallize the compound, freeze it out of the mother liquors, subject to vacuum filtration, washing with first ice cold water, then with several portions of acid, and enough further portions of ice cold water to remove the acid (the acid washes were to remove the catalyst) and return it to a neutral PH, more vacuum filtration and sucking the cleaned intermediate bone dry in a buchner funnel at the vacuum pump until dry as dust, light and fluffy.
Then a reduction and three-step purification, finally distilling off the solvent to leave the second intermediate.
To go, the very last of the intermediate steps, a vacuum distillation followed transforming that last product into another, penultimate intermediate compound, purifying it and finally arriving at my desired end by means of a reduction using a modified sodium metal-based reduction technique, with a wee adaptation of my own.
So, after all that work, I am rather pleased and satisfied with myself for all the effort I put in so far, to see my second-to-last intermediate product sitting there, gleaming prettily back at me, as if a newborn child, with just a little bit of further growing to do before its finally ready to say its first words, so to speak
What are you aware and thankful of my lovely?
