posted 01-16-2000 11:15 AM         

1. I used lab grade chem. so if your receipe called for 70% alcohol I added water to my 99.9% alcohol. Correct?

2. In the 2 step my yields were too high, but tests you suggested checked out. Too much of something left in by me?

3. After step 3 is done and the rxn is flooded. Should the (I'm guessing benzo) black crystals be kept as part of the aqueous layer and washed with 2xdcm?
I have done this one 3 times I'm imbarased to say, with the same results. Some say filter off and wash but I'm guessing there is product in it. One try netted 12g.in step 4

4. Step 5, dissolve 50g.MethylAmine in 91% alcohol(this is why I think my step 2 was wrong, mine would not dissolve) And all of the Al did not get consumed.

5.I'm doing on a very personal scale so fortunately have not lost much product yet. It is O K to scale this down, right?

6. Step one was done 3 times but with my aspirator I'm not sure if it is good enough. All three times got product at 204c.
I think this is ok (product was water white and refracted light)but if I cant get the vacuum down then how will I collect product from step 4 as the temp + 25 = 229+-
Is my vacuum no good? (it is new) I suspect the thermometer adapter is the weakest link(a rubber boot over an adapter seems like a possible leak to me!) in the set up but I have not a clue if it is failing somewhere. Is there a way to know this? Are metal clips better for this?

It SOUNDS like the vacuum is working( there is a point when the pressure builds to stop the water flow to a tickle) but having never done it before I have no idea if it is. You see?

Please have mercy on this wanna-bee
Your help is greatly appreciated.
I've heard it said that this was easy and out of all the recepies this one does sound the most simple. Thanks for all the work you ALL have done here.

posted 01-17-2000 09:00 AM         

Just know that you are NOT being ignored.

posted 01-19-2000 07:50 AM         

1. Yes ... To make 70% from ~100% ... 70mL of ~100% + 30mL of Water ... Ta-Da.

2. More than likely, you have Ammonium Chloride mixed in with your MeAm.HCl. This is not so bad ... Ammonium Chloride will not react quite as readily with your ketone in the Al/Hg .... So ... basically add 120% of whats called for (of MeAm.HCl) in the Al/Hg. This way the excess of MeAm.HCl won't hurt and the Ammonium Chloride will be reduced to a bi-stander. Besides, Ammonium Chloride should theoretically produce MDA, which is completely psycadelic as it is ...

3. The Crystals are actually hydroquinone ... In Reduction/Oxidation reactions, one compound is always oxidized and another is always reduced. The saf is oxidized to the ketone, and the benzoquinone is reduced to hydroquinone.
You are correct though ... there is a little product sticking to the crystals ... after you flooded your mixture with the HCl solution, the oil drops out, you wash the solution with DCM to get a little more suspended product ... Now, theoretically you can add a 25% NaOH solution (SLOWLY) to the acid wash to make it basic ... this will keep the hydroquinone in solution, Wash again with DCM ...
But to be honest with you, the best plan is to upscale. If you do it on the scale recomended in the procedure, you will get much more ketone than that ... and it will pop right out of solution and you won't have to really work for it. Don't be scared of the larger quantity, think of it as 'product insurance'.

4. Interesting. Did you hold the temp at 104C in the MeAm.HCl procedure? That 104C is very important. You must hold it at that temp for as long as the directions say ... The MeAm.HCL will go right into a 91% solution ...

5. I wouldn't do that ... for reasons explained above. Now, I think that the hardest part of the synth is the Al/HG procedure ... Its not that hard, but many bee's have problems with it. You can make alot of the 'ketone' and then scale down on the Al/Hg ... so you get some practice ... That would be fine ...

6. Yes, that aspirator sucks (or doesn't suck ... hehe). You need to look at your hoses, and your connections. You need to make sure there are good seals formed everywhere ... And turn up that water!
If your Safrole came over at ~204C ... then your ketone will come over at ~230C ... well above the scortching temp. You need to have your saf, come over around ~150 or lower. 'Not-me' has an aspirator that pulls saf over around ~120C ... so it is possible.
To check your aspirator, turn the water on full blast, and put your finger over the suction port, and feel the vacuum. Two things should happen:
1. You should feel a 'good' vacuum.
2. The water spraying out of the end should change sounds. <- Thats not clear I know... but if you try it you'll see...

Things to fix it ...
1. Attach a hose (thin guage) to the end of the aspirator (where that water is exiting) ... Sometimes a longer hose will produce a better vacuum....
2. Connect all your hoses with a little Vasiline as a lubricant ... This will help to seal all the hoses ...

posted 01-19-2000 06:50 PM         

2. What color is the organic layer of oil just below those hyroquinone crystals after the wacker is flooded?

3. After the oxidation has completed, is the mixture more liquid now and back to room temp?

I'll bet you did great on you exam!
Thanks very much for your help Bright Star.

Able to Dream Again,
DeJay/