02-14-02 00:31
No 269321
got a few questions out there if anyone is out there.
In the Brightstar write-up there seemed to be some problems
chromic was helping me work on but Im lost.
use a 1000ml rb flask
use 100g MeAMm.HCL disolved in 100ml h20 and slowly added
60g.NaOH disolved in 180 ml H20(use icebath)
1.At what rate do I need to do this addition?
2.how do I do the addition?threw use of add/sep funnel
or should I use a dropper?
Then in a 1000ml flask add:
650 ml MeOH,0.2g HgCL2,40g al foil.
let amal.till bubbles appear on foil surface.
3.Do I need to rinse off the foil?
4. how long does it take for this too happen 30 min?
Then add MeAM solution then 80g MDP2P.
5. just add the two back to back,dump in?
Let run 5 hrs with external heatkeep light reflux.
this means what?just before steam comes out the mouth of column?
Then extracted with tolly,washed tolly with water,filtered tolly,washed again ,then dried ,and gassed.
This was pretty vague.
I will choke untill I swallow!Who are you to judge or strike me down!
(Hive Addict)
02-14-02 01:06
No 269332
>1.At what rate do I need to do this addition?
>2.how do I do the addition?
Just slowly slowly pour one into the other (a couple minutes or so) with gentle stirring in an icebath.
>3.Do I need to rinse off the foil?
>4. how long does it take for this too happen 30 min?
Don't rinse off the foil with this method, takes about ~20 minutes. Bright Star likes to prepare the amalgam then wash it, I personally think it's harder to do it that way.
>5. just add the two back to back,dump in?
Yes, just dump them both in.
>Let run 5 hrs with external heat. keep light reflux.
>this means what?just before steam comes out the mouth of column?
Basically, I just let it run, it should stay at a low heat then start to cool, when it does, throw up the tempearture to bring it up to a light reflux and use up all of the foil...
>Then extracted with tolly,washed tolly with water,filtered tolly,washed again ,then dried ,and gassed.
>This was pretty vague.
There's other workups you can use. I don't like how Bright Star extracted with IPA, I think it's better to do it with toluene (like how MM worked up his reaction). Filtering the toluene seems to be the fastest way to clean up the toluene for gassing.
(Newbee)
02-14-02 01:16
No 269343
Addition of NaOH should be relatively slow. There's no set amount of time, just don't let it get out of control. All your doing here is freeing the MeNH2, so the speed is fairly irrelavent. Just don't make a mess.
Seperatory funnels are great for this. Just start it out on a slow drip.
Some have said that you can get better results from washing in NaOH solution for a few minutes. I did, and my results were okay. I'm not sure if it helped, but it couldn't hurt. It should take about 20 to 25 minutes. Could be slower or faster. Just look for the things BS talked about. You might look at PIHKAL #109. That's where Brightstar got his idea.
At that point, just add in you ketone and MeNH2. It should be immediate, so yes, just add them back to back.
Light reflux just means not too vigorous. If it's going clear up the column, then your one step from taking a bath and lossing your product. Keep an eye on it and make sure your water is cooled if it's not tap. It traveled about 1/4 to 1/2 way up the column when I dreamed about it most recently, and that made me nervous. Your just going to have to sit there and watch it. Don't use the addition of heat too quickly. Take your time.
As far as gassing. We'll I've never done it. It doesn't sound hard. Just follow the gassing methods you find here. I've seen several references in the last couple of weeks, so information on gassing is easy to get. Just use the search engine.
(Hive Bee)
02-14-02 20:51
No 269734
Thanks for all of your help!I think Im finally about to
have a lucid dream.
I will choke untill I swallow!Who are you to judge or strike me down!