Please review what i have done and please tell me why i had some troubles.
I started with 500 ml rb flask my fisher 7" aluminium plate, a bowl with peanuts oil and a water aspirator ( plastic one ).
OK OK i started the aspirator and i turned the heat and of course i had boiling stones.
After almost 1 hour the temp didn't want to go upper than 42 degrees C.
I paniced then i got rational again, i turn the water more on... but nothing... so i placed my stir bar in and got it spin at warp 5 but still no more than 42 C.
Then i wrapped the flask and bowl with aluminium foil and waited... a little ... but still nothing... so i put the heat at maximum (10) and after a while the temp climbed and at 110 C some white like water stuff come into the reciving flask... but the temp climbed a lot.... so i turned down the know to 8 but nothing... it was approching 170 C so i took the aluminium foil off and it went down.
To make it short i have tried every way to stabilize the temp but it just didn't.
I have noticed that at 10 the temp after 10 minutes got up... i have noticed that by turning off the stir bar the temp goes down... i have tried to set the temp of my fisher at 8 or 7 but the temp goes down.
So i was unable to stabilize the temp it either goes up or down...
the flask was immerged almost half into the oil and 1 cm of sassy was above the oil level at beginning.
The safrole i have gotten is clear like water it smells more softly but somehow different than sassy and it reflects light with some mild yellow/green shadow ( but to see this shadow i had to put the bottle against the light ...).
My concern now is step 2... how am i supposed to stabilize the temp at 104 ?????
Please tell me whatever i did wrong so that i can correctly tomorrow when i start step 2 and 3 .
Thanks guyz.
Andrew
As for temp control in the methylamine synth, you don't need a second stir bar in the oil. Just stir it by hand every now and then. And it is a good idea to put a second thermometer in the oil. You raise the oil temp to ~104C, wait ten minutes or so then check the temp in the reaction flask. If it stops rising and is below 104C, then raise the temperature of the oil by a few degrees. Check the reaction vessel temp again...repeat until it hits 104C.
....or you could by a mantle on ebay for $20 (https://www.thevespiary.org/rhodium/Rhodium/hive/hiveboard/picproxie_docs/000104837-file_n5ac.gif)