iso help required

bigwhisky · Wed Jun 22, 2005 4:48 pm

bigwhisky is dreaming of creating some iso so has had a look at a few synths.
bigwhisky dreams of doing this in the shortest possible time period so has all but ruled out the strictly KOH method and instead is looking at a method using a solvent, I thinks ethanol from memory.

Also, is bigwhisky correct in thinking that the method as appears is TS2 using Cao has been rejected.

If anybody has some pointers on iso synths they would be most welcome.

thanX,

Bigwhisky

Soap · Thu Jun 23, 2005 5:25 am

well swim has never used the Caoh method but heres moderate things about it. swim believes it take around thirty minutes, but yeilds are lowered if theres no vacuum filteration at hand. i have heard of people doing it strictly with koh at higher temperatures in no more than 2 hours, though swim has never tried it himself.

MAKE SURE THAT SAFROLE IS CLEAN!!!!

ApprenticeCook · DILLIGAF

Make sure the safrole is double distilled and pref before that you could also freeze it twice (search for the threads on safrole freezing) then just use the KOH method, you can use EtOH solvent as per the data tables on the rhodium mirror and see how u go.

-AC

2spun · The Resistor

swiy has ,

double'd distilld and then used the KOH/CaO-iso method ran it 2hrs,4hrs, and all inbetween same outcome." cold cold water in the condencer please.
swiy lost oil. maybe 10-15%,
now swiy can't speak for all the oils out there and the means to filter.
but swiy would surly use vacuum filter to get the most back.
Much thanks

ps

swiy has heard that the KOH method works well but w're look'n at 12hrs plus?
maybe wrong. maybe longer? "swiy belives temps have something to do with this"
swiy not 100%
swiy wood think it's up the swim. what he's will'n to go for and/ are will'n to loose. or gain.(depend'n on ones oil) "from what swiy understands"
that mean'n there is more than 1 way to make iso and by the means that swim has at hand and his exp.. in geting back what she has labor'd for.
all respects

ApprenticeCook · DILLIGAF

plain KOH is left to go for it overnight, says measurements were taken and it looked as thought the reaction had completed after 5hrs but leaving it over night just makes sure it gets done as far as it can.

-AC

bigwhisky · Thu Jun 23, 2005 4:13 pm

When one says overnight are we talking a 16 hour window or perhaps something smaller, are time periods needed for the iso to form temp dependant?

thankX,

bigwhisky

bigwhisky · Thu Jun 23, 2005 4:25 pm

Isomerization of DISTILLED 1-alkene with 1% KOH CAN be done, according to SWIM with >90% yields in under thirty minutes @ 243癈.

Experimental: Dissolve using heat and good stirring 1 gram of KOH in ethanol of methanol. Once dissolved, add 100 grams of DISTILLED 1-alkene to mixture and increase heat to distill off the alcohol, which can be reused. Place thermometer in flask and continue to heat and stir until temperature reaches 243癈 (it will hit 232癈 first, linger awhile, but will soon ascend). Hold for 5 minutes, the turn off heat and let cool. Next, vacuum distill to get desired product.

If dirty 1-alkene is used, considerable tar will form, covering up the KOH (making it inactive). Also, the stirring will be slowed immensely. Up to 500g of dirty 1-alkene was used. Stirrer stopped at one point but continued heating and refluxing ensured relatively complete conversion into the 2-alkene. For odor control, a dampened paper towel was lightly stuffed into the opening of the flask. Keep in mind that the cis-isomer of the alkene in question boils at 245癈 at normal pressure. The trans boils at 250癈 or so.

Ripped this off the Rhodium page. any thoughts on this one?

thanX,

bigwhisky

ApprenticeCook · DILLIGAF

"1 gram of KOH in ethanol of methanol"
Huh?

Its a simple process well covered already resulting in the large review document being published on rhodium. I dont see why were all still talking about it, each of the methods on the review page work exactly as described if conducted exactly as described.

-AC

bigwhisky · Tue Jun 28, 2005 4:44 pm

The above method does not appear on Rhod Iso Synth page. The above synth appears tucked away at the bottom of a ketone synth using Oxone as presented by Chromic, on Hot Rhods site. All the way at the bottom. Maybe for good reason? Hey but that what i am trying to work out cause it sure sounds good. Comments??

'ethanol of methanol'- methylated spirits i am tipping

thanX,

bigwhisky