Возвращаясь к нашумевшей статье профессора Томаша Худлицкого
(https://vk.com/himik_psihopat?w=wall-29287308_468306), которую "изъяли" из интернета. Абстрагируясь от различных неоднозначных моментов, помимо всего прочего там есть интересный для любого синтетика момент в сноске номер 6. Там он говорит о том что его наставник в 70-х года научил его как можно перегнать 3 мг вещества и что сейчас эта техника позабыта.
Мне стало интересно как такое действительно возможно и я не нашел иного варианта как просто задать этот вопрос автору статьи. Ответ пришел в течение часа. Ниже прилагаю оригинал. Возможно кому-то эта техника пригодится.
I was a postdoc in Geneva , 77-78, under my “Master”, Professor Oppolzer. I had ~3 mgs of a viscous oil, precious intermediate (14 carbons) in my total synthesis of isocomene. It was maybe 85% pure and he wanted a combustion analysis and told me to distill it and submit. I said that you cannot distill 3 mgs. He got angry, cleaned my bench and showed me. I was speechless…
He put water in the beaker to warm up on the hot plate. Then he took a soft glass tube and with a Bunsen burner sealed the end and then blew a little side bubble about 4 cm up the tube. He then put the tube in the beaker of water, with the small bubble facing up. Dissolved my stuff in ether, took it up in a pipette and slowly ran the solution down the side of the, now warm tube. In a few minutes, the ether was gone and there was, quantitatively transferred, the 3 mgs, of oil in the bottom of the tube.
He then attached a hose to the tube, connected directly into high vac pump, and slowly passed the bottom through a soft Bunsen flame. This time, the side bubble was pointed down. You could see the oil slowly crawling up the side and collecting in the side bubble, when it reached the edge of it. Took maybe three minutes. Then he adjusted the flame and sealed of the side bubble into a tear droplet. In it was the clear oil. He gave it to me, gave me a “look”, and said “Zis vil analize!”. Walked out.
A True “master”. I have taught this to many, many students. How many people today know such techniques??
