bbeeasheets (Hive Bee)
10-07-04 16:01
No 534870
       Safrole isomerization under vacuum     

ok, i just purchased a sargent-welch 1405 duo seal vacuum pump. unbelievably to me, it distills safrole at 64C! (100 degrees lower than my last pump) my question is, i prefer to isomerize under vacuum (i heat to just boiling, but where it doesn't distill), and when boiling ceases the isomerization is complete. Will safrole isomerize (with KOH) at 60C? 		 
 
 
 
    Rhodium
(Chief Bee)
10-07-04 19:04
No 534886
       Too strong     

At 60°C the isomerization will take days, if it at all will go to completion. Use another pump or use a bleed valve with this one (something as low-tech as a leaky rubber tube is fine, adjust the vacuum by pricking holes into it with a pin).
The Hive - Clandestine Chemists Without Borders 		 
 
 
 
    ApprenticeCook
(Hive Addict)
10-08-04 01:33
No 534931
       all the vacuum is required for here is to...     

all the vacuum is required for here is to remove excess water as this is a killer, but rhodium is right i use my aspirator... or just put deliberate leaks in the system you have.... but thats a nice pump for disto, good on ya!

Hey just a question from me....
Is there some relationship table/grpah around that has the isomerisation rxn times vs temp??? just so i know what the ideal temp for the rxn to be is to achieve the better yields....

-AC
Its just my opinion, but no-one listens to me anyway, and rightly so... 		 
 
 
 
    abolt
(Hive Addict)
10-08-04 01:48
No 534936
       HMMMMMMM     

The best kind of pump for isomerisation is one of those shitty teflon membrane pumps that pull 20-25" hg.wink
THEY GIVETH WITH THE LARGE PRINT,and taketh away with the small print


 		 
 
 
 
    hypo
(Balanced Ego)
10-08-04 02:34
No 534941
       hmmm...     

is that 20-25 inch or mm?
if it's 20-25mm Hg, i'll take your "shitty" pump! wink
"And you for sure cant read nor write assembler, idiot." - orgy. 		 
 
 
 
    abolt
(Hive Addict)
10-08-04 02:40
No 534943
       Ça Plane Pour Moi     

(')= feet
(")= inch

25' would signify 25 feet
25" signifies 25 inch

Yeah, yeah I know.........I'm supposed to (Use metric units)

When I can find a mm/hg vacuum gauge for less than $2,000, I will throw away the old in/hg one. (sources welcome, please P.M.)

thanks for bringing it up, hypo
THEY GIVETH WITH THE LARGE PRINT,and taketh away with the small print