nigl
Rising Star
So I had some freeze precipitated yellow-lightbrown spice which I wanted to purify and crystallize.
About 1.8g of the product were placed in an erlenmeyer and with 50ml Naphtha (Pentanes, Hexanes, Heptanes) and put on the waterbath at approx. 60 °C. The solution was stirred until more and more yellow product was solved in the liquid. A brown goo didn't go in solution and was filtered off (the filter was washed before with hot naphtha too prevent the product precipitating in the filter). A yellow clear solution was obtained. The dark goo in the previous flask was washed with 20ml hot naphtha again and the combined naphtha solutions were put in a crystallizing dish.
Now I know this is technically not recrystallizing but after letting the solution sit overnight at room temperature there were some very nice 2-4mm crystals visible and also some 1mm diameter orange drops. When all the naphtha has evaporated and only crystals and drops are left I could simply carefully take the crystals and wipe the orange oil with paper. I can't get all of the oil but after that I can do a real recrystallizing step when I have much less oil so that it won't precipitate like it did this time but rather stay in solution.
What do you guys think?
About 1.8g of the product were placed in an erlenmeyer and with 50ml Naphtha (Pentanes, Hexanes, Heptanes) and put on the waterbath at approx. 60 °C. The solution was stirred until more and more yellow product was solved in the liquid. A brown goo didn't go in solution and was filtered off (the filter was washed before with hot naphtha too prevent the product precipitating in the filter). A yellow clear solution was obtained. The dark goo in the previous flask was washed with 20ml hot naphtha again and the combined naphtha solutions were put in a crystallizing dish.
Now I know this is technically not recrystallizing but after letting the solution sit overnight at room temperature there were some very nice 2-4mm crystals visible and also some 1mm diameter orange drops. When all the naphtha has evaporated and only crystals and drops are left I could simply carefully take the crystals and wipe the orange oil with paper. I can't get all of the oil but after that I can do a real recrystallizing step when I have much less oil so that it won't precipitate like it did this time but rather stay in solution.
What do you guys think?