07-20-02 08:16
No 334953
What happens when you add the safrole all at once in one of these rxns. I know someone has tried this, so how did it go??
VL_
(Hive Bee)
07-20-02 08:35
No 334958
Shit yields is about it.
(Hive Bee)
07-20-02 12:02
No 335005
Yes once safrole is introduced the reaction between the catalyst quinone and safrole beign. If you want good yields drip it in over two hours for 200g batch and let it stir and reflux for 8-10hrs. Gives 180g ketone consistantly plus some isosafrole if you have good fresh p-benzo.
(Hive Bee)
07-20-02 20:49
No 335133
Still too proud to spring for that addition funnel huh?
(Hive Addict)
07-20-02 22:13
No 335150
So far swim hasn't needed one. Hell swim went fishing yesterday and fished with a string and a hook. No pole. ANd he caught more fish than anyone on the river.
VL_
(Hive Bee)
07-20-02 22:39
No 335164
This reaction provides very good yeilds, and is much more expedient than the isomerization > peracidic > hydrolytic rearrangement, as well as less prone to error. In itself a reaction as beautiful as this one is worth the extra money spent. Organic peracid synths are ghetto and only need ghetto equipment. You should do this reaction justice. I think you should go ahead and buy one, man. It would keep you from having to sit over your reaction adding small amounts for hours (although just sitting and watching is a lot of fun). It would save time and trouble and increase your yeilds, while you could just be chilling out smoking some nice reefer elsewhere. Sounds like a good investment for the money and would also make those aminations a lot easier.
Flip
(I'm not Cheesie)
07-20-02 23:04
No 335179
Anything's better than Oxone as a peracid, what a joke that turned out to be.
Bubba Fatt - LA's Biggest Bounty Hunter. His subjects are at large and so is HE!
(Hive Addict)
07-20-02 23:50
No 335204
Could you seriously not get the oxone to work. Commercialy available Potassium persulfate might solve the volume efficency problem withthe oxone route but then it would no longer be an oxone route.
Swim is willing to run an experiment to see exactly how much safrole can be oxidised with 2 grams of PdCl2.
He has a few q? though.
With the typical ammount of Benzo(150 gms) how much safrole could be oxidised if all the benzo gets degraded to hydroquinnone.
What is the typical % of benzo left in a 1xmmbenzo wacker
?
(Hive Bee)
07-21-02 01:49
No 335260
In SWIMS experience all benzo apears to get used and converted to hydroquinone. Though SWIM usually got his pd back by solvent washes and electrolysis but the returned metal is worth less than the chemicals and electricity used so it was a waste. He usually gets back a mixture of safrole and a lil eeny bit of iso also. So i would guess that means if extra p-benzo were used he would have gotten no unreacted safrole back. Why go through the trouble of finding out when it has already been done? Rhodium or osmium were in the conversation and gave the technical info on how much benzo extra was needed for the scaled reaction and the theoretical max for the 1 and 2g pdcl2 batches. I remember someone doing the eact same reactin jsut using like 1 or 1.2 or something under 1.5 g and jsut reacting longer and got about the same yield. I believe the max was found to be 200g for 1.4g and like 400g for 2.45 or soe shit likethat I'll try and dig up the thread tonight.