TheHobbit (Stranger)
06-19-03 18:56
No 441181
      Ketone Problem  Bookmark   

I used the TFSE but I only found one helpful post relating to my topic but it didn't answer my question.

What about this seems wrong:

Safrole came over from sassy at 135-140 so you know the vacuum strength.

The p-benzo reaction was pretty messy but once cleaned swim believe he actually had p-benzo, it was deeper orange than anyone on the board said it would be though.

Swim did methyl mans benzo waker to produce his ketone.

Upon washing the reaction swim would get a LOT of gunk on/in the aqueous layar. Swim made sure to keep it out of his dcm/ketone layer.

In the writeup it says when you start washing with NaCl and NaOH you should see green overtones in the dcm/ketone. Swim didn't.

After all washes were done the ketone/dcm layer was a deep red color, no green overtones. However it was pretty transparent as opposed to when swim started. No scum was in it.

Swim distilled off the DCM.

Swim started to distill again for the ketone. Swim added about 1 oz safflower oil as a buffer which swim has now read it unnecessary.

Swim forgot to put the vacuum hose on to begin with. So when swim did, immediately some safrole came over, very little, maybe 10ml, 15ml at the max.

The safrole came over rather fast and condensed rather fast. After the safrole was all over there began a slow drip. It was bright yellow.

Swim thought it could be ketone at first so he went to sleep and let it distill. When swim wakes up there is maybe 35ml of solution in the receiving flask including the safrole.

Swim let it boil for over 8 hours. Nothing more in the receiving flask. The boiling flask still has a lot of solution in it, I would say about 130-140 ml, maybe upwards of 200 ml. It is deep red, almost black. No thickness of polymerization.

The oil temp is a little over 200, maybe 210. Oil is peanut oil.

What is swims problem? Swims ideas:

Bad benzo, the excess amount of sludge between layers could have meant way too much hydroquinone left in the reaction, even after filtering.

Temp still too low? The hot plate is working fine, getting hotter than 200, not sure why the oil hasn't raised above that after that long of boiling.

Something else went bad in the rxn.
06-19-03 19:31
No 441189
      dont go over 200, get a better vacuum source,...  Bookmark   

dont go over 200, get a better vacuum source, recrystal your p-benzo in either IPA or methanol ( correct SWIM if there wrong) Ketone should come over around 170 in your case.
06-19-03 20:37
No 441200
      Well, I am not 100% sure it is benzo.  Bookmark   

Well, I am not 100% sure it is benzo. I washed with ice cold IPA and recrystalized by evaporating then excessive cooling to get pretty pure looking crystals. I think the vacuum should be enough to pull it over at 170-180 like you said, so I honestly think I just fucked the reaction up completely.
(Hive Bee)
06-28-03 12:06
No 443147
      make some pbenzo  Bookmark   

Why are you using a chemical that you are not 100% sure what it is? Good p benzo will be yellow, not orange. I recommend making your own p benzo for two reasons. 1. It's safer than buying it or using unpure "p benzo." 2. It will give you more pride to know that you synthed one of the precursors. There are several posts on Rhodium's site on how to make it. Bee sure to make it right before you need it, so as to battle decomposition due to light and air. good luck peace

D.A.R.E. = Drugs Are Really Exciting
06-29-03 00:15
No 443229
      I did synth the p-benzo, if you read above I...  Bookmark   

I did synth the p-benzo, if you read above I said that reaction didn't go as planned an resulted in way orange pbenzo. After recrystalization it did come out more yellow but it wasn't benzo. Since then I did figure out what I did wrong in the benzo reaction.