what color should the xylene extractions be? mine came out light purple!?!?!?Never judge a reaction by it's colors.
kept going and xylene got really cloudy (but didn't see any crystals) so kept gassing, then this brown gummy goo formed on in the xylene. This is because your product is not properly cleaned. Yoou should do
at least, a full A/B cleanup of your amine before gassing. UTFSE to read up on A/B washes.
If you expect decent answers, you should give decent info.
Was your ketone tested?
Was it properly distilled?
now i have this brown goo and the xylene got a lot darker in color too.
took out the xylene, washed with 2x dH2O, 1 saturated baking soda, 1 saturated NaClYou washed the Xylene again, after gassing? If you did then most of your product is most likely in your washes.
i've read that what happened was overgassing.The chief has stated that "overgassing" is a fallacy, I agree. The brown shit you had most likely had some amine in it, that was very dirty due to the fact that you didn't purify it properly. Hence, the brown color.
Can anyone help me out here? second dream is about to come and need to know if the old xylene is salvagable or just start again!?!?If you washed again after gassing then the product would be in the first of your "2 x DH2O washes".
Evaporate the water, dissolve the left over sludge/crystals with strong NaOH solution, extract with fresh xylene, wash 3 times with 5% NaOH and discard washes.
Then make acidic with 10% HCl, tap off the lower water layer and place the xylene aside. Now wash the acidic water with 3 x equal volumes of fresh xylene and discard or recyle xylene washes.
Now you can either:
1. Make basic again with strong NaOH solution, extract with Xylene, dry with MgSo4 and gas.
Or better yet:
2. Make basic again with strong NaOH solution, extract with Xylene, distill away the xylene and then distill the freebase, place distilled freebase in fresh xylene, dry and gas.
The very best advice I could give you is that you need to do a lot more reading before commencing again.
.........or you will keep having nightmares