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Curbshot Nano Redeux...

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mickyfinn:
Well, they say that the third time is the charm...(whoever they is)

1G E
2G MBRP
3G i2 crystals
125ml pyrex rb flask
small crock pot with sand inside

Ingredients went in according to the curbshot spec, the ballon was taped and the flask shaken well (with a finger covering the flask opening with the balloon.) Immediately, there is gas in the balloon, things bubbling madly in the flask which is then set in the sand inside the crock pot.

PROBLEM? The sand was not hot yet....will this ruin SWIM?

A towel is used to cover crock-pot replacing the lid since the top needs to accomodate the flask and balloon....but it doesn't seem to be bubbling like mad, if at all, as it was initially. It has been 10 minutes and the unit is now heating the flask....SWIM remembers post by O that visual indication is not necessary for a reaction to occur.

Is SWIM screwed, blued and tattood? SWIM gonna go kissin' a movin' train if this one fails....

Quick peak at small part of flask under towel reveals no perceptible activity. However, what can be observed of the fluid along the interior looks like candy apple red on a corvette.

Help SWIM Obie Wan Kenobi, you're SWIMFINN only hope....

Osmium:
I hope you will enjoy your iodometh.

mickyfinn:
I hope you will enjoy your iodometh.
--- End quote ---

SWIM glad Crotchety Obie Wan make fun of newbee SWIM... Bad Obie Wan...newbee clearly unmatched and easy target. WTF?

Got the drift and point (although wrapping the present in a wad of GAAK verbage leaves something to be desired.)

For anyone interested in helping newbee to dream first dream...the balloon swelled to double 1 hour into the reaction. SWIM pinched the balloon and slipped thumb over most of opening...then added 3-4 drops dh20 to the rxn and (OMG what the smell of that smoke is nASTy) re-attached the balloon without losing any (hardly any it seems) of the ballon contents and returned to crock pot sand bath.

SWIM wants to follow the post reaction workup by geezer and could use some indication from experienced bee as to whether this is a good idea and whether the addition of the 3-4 drops dh20 was enough...hope so as I'm off to sleep...but first...

Searched for iodometh and found present in snide comment...so a thank you to O is in order.

Thanks

Jetson:
they,  heh.  swij knows they.  but anyway...  jetson used to fuk with small nano's all the time(probably still does according to some bees standards,  under 10g=nano?)  and has found that small rxn to be inconsistant and therefore has scaled up a bit.  it's sometimes hard to tell if it went at all or is just burning away from the heat.  the only thing you can do now is to work it up and see what you end up with.  if your balloon swelled to double the size then swij would probably bet on conversion.  he's never had a balloon swell up past the initial standing up straight of one and has had some verry nice nano's.  just work it all up and keep your fingers crossed.  if you have decent lab techniques then you should end up with something.  at that small of a nano though one shouldn't put too much work into it.  may jetson suggest scaling up slightly?  it'll prove much easier to follow the rxn and easier to work up.  well good luck there mf.  oh and don't ge smelling the fumes and tell they to piss off....   they're always doing something to try and keep a bee down...

Osmium:
> 1G E
> 2G MBRP
> 3G i2 crystals

Since you want the reaction to take place in strong, aqueous, about 55% HI I'd say you should have added about 1-1.5ml (=1-1.5g) of H2O at the beginning.
Since it is probably too late and that much water might quench the reaction since most of the I2 has already reacted I'd add about 0.5-0.75ml of water and hope for the best. Since you used quite a lot of I2 the conversion of the precursor and the final yield should be pretty good.

Next time you do such a reaction add the pfed + rP to the flask, followed by the water, and then add the I2 in 2-3 portions. No drama, no gas losses, a quiet reaction, and after a few hours reflux you're done.

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