P-benzo wacker failures...Help

[FlaskGenie]

This is my first post so I apologize in advance for my newbeeness.  My dreams lately are disturbing, almost nightmares.  I dream all night long and just before I wake I am rewarded with just a drop or two of very cool lime green minty fresh liquid.  Three failures all ending the same.  Tiny black globs in distillation flask.  It is the standard benzo the small man performes in my dreams.

50 ml Safrole (dist @146c w/ refrigerator compressor)
20ml Nitro     (from Rc Fuel)
25ml Meoh    (from Rc Fuel)

60gm p-benzo
1.1gm Pdcl2
200ml Meoh (from auto store)
25ml Dh2o

Compressor checked out w/ vac tester from auto store at 30”

Between the three dreams there are some variables but there are similarities.  In none of the dreams was the post benzo DCM/oil washed with anything after Naoh washes.  If someone could tell me at what temp Naoh polymerizes I would be grateful.  Also I have read that some bees who pull safrole over at 120c don’t pull keytone till 160c.  If that is the case I think I may have a vacuum problem.  If anyone is interested I can post the full lab notes of the three failures.  I am reluctant to proceed without guidance.  Also if a bee out there might have suggestions for preferences on a vac pump I would be grateful.  The few drops of keytone I do get is through simple distillation.  Can’t pull keytone over through a fractioning column.

Do I have a Naoh problem in post wacker distillation?
Do I have a vacuum problem?
Is refridg compressor at 30” strong enough to pull keytone.
I am confused by all the different advice for washes.

Thanks in advance

[homeslice]

Also if a bee out there might have suggestions for preferences on a vac pump I would be grateful.

I'd recommend a ritchie 4-6 CFM vacuum pump on our favorite auction site, it works nicely.
As far as everything else goes i'd rather let more elder bees comment. Failing 3 times already w/o asking any questions prolly wasnt a good idea. The black globs on the distillation flask sounds like charring, at what temp was the green shit comin over at?

Swims safrole came over at about 100c with a ritchie, 146 sounds really high.

[Belial]

>50 ml Safrole (dist @146c w/ refrigerator compressor)
>20ml Nitro     (from Rc Fuel)?!!!!
>25ml Meoh    (from Rc Fuel)

Although so many things could be responsible for fuckups, perhaps you should start with the obvious improvements, e.g removing reagents from the reaction that are not meant to be there!! e.g. Ditch the MeNO2!

OR if you have your heart set on using the MeNO2, send me all your Pd, you wont be needing it.

[pickler]

Don't know what your doing with the nitro, But for a benzo wacker you only need pdcl2, meoh, safrole and benzo. When it's finished do 3 salt washes and 3 baking soda washes. With each wash you should get less and less crud from your ketone layer. Then wash with naoh. Wash until the naoh water is a lighter orange then do a water wash or 2 on your ketone layer. Swim has had the problem your talking about many moons ago. Apparently  from not washing  the ketone layer good enough. Make sure to use the correct amount of dcm when taking up the ketone layer. Your ketone/dcm layer should be very thin like water. If it's the slightest bit thick it won't get washed properly. When distilling your ketone turn the heat up slowly. it takes awhile, but your patience will pay off with lots of yummy ketone!

[Mercury]

C'mon man, you need to do some more reading as it's clear you fucked up the synth long before you even got to the washings. You were probably reading MM's p-benzo wacker and Al/Hg amination at the same time and got fucked up along the way! Were you drunk or something? HAHAHAHHA

I'm no chemist, so perhaps someone else can explain what affect the nitro would have in a p-benzo wacker. I can't see it producing any benefit to the reaction, that's for sure.

[FlaskGenie]

Thanks go out to the hive for all the input.  I am humbly grateful.  I apologize for the ambiguity.  There is actually no MeNo2 in the wacker phase.  In  three dreams I managed to pull over 4.5 gms of keytone which I proceeded to fuck up.  But first things first.    The green stuff came over @ 165c to 180c w/ more coming over closer to 180c.  The small amt. came over right before the black globs appear.  Can you do too many washes? Swim is now a washing SOB.

[Mercury]

Why do you neglect the NaCl wash? I'm assuming the only reason would be that you can lose product with this wash.

[Rhodium]

NaCl washes generally bring about emulsions that withhold product.

Oh? In this particular synth only then?

Myself I usually add some conc NaCl solution to an extraction mix when I want to break an emulsion...

[pickler]

If your not using enough dcm for your organic layer, then yes the washes will hold product back and lower yields. Swim speaks from experience with this. Use the right amount of dcm. It looks like an overkill, but it is needed.

You could very well have a leak in your setup. silicone grease is the best. They carry it at the auto parts store. Go get some. You might want to look into a better vacuum source too.

[pickler]

If your not using enough dcm for your organic layer, then yes the washes will hold product back and lower yields. Swim speaks from experience with this. Use the right amount of dcm. It looks like an overkill, but it is needed.

You could very well have a leak in your setup. silicone grease is the best. They carry it at the auto parts store. Go get some. You might want to look into a better vacuum source too.

[Mercury]

I heard other bees saying that Vaseline works well to grease joints. Does it liquify under high tempurature?

[Just4Fun]

FlaskGenie, What type of compressor are you using?

[FlaskGenie]

To Justforfun.  I am useing refridg. comp.  vac tester says it gets 30"

[FlaskGenie]

I have tried vasaline and it does not work well for me.  Am useing High temp auto brake lube.  Its blue so you can see it in the joints and it stays in place w/o breakdown to 200c in my dreams

[Chromic]

SWIC uses some lip gloss stuff. I don't know what the fuck is in it, but it's good until at least 300C. It's better than vaseline or anything I've found so far (that will just turn to a liquid and flow out of the joint)... its probably at least comparable to corning's high vacuum product and it smells like bubble gum. I wouldn't recommend it or whatever, but it was perfectly OTC and works just fine for SWIC.

I guess SWIC is one of the few who gets away with it.

Btw, it's extremely hard to keep a fridge pump in good shape unless you've got a good trap. Good luck!

I have no idea if SWIC will be smiling in the end. I would only wish him the best in life.

[Mercury]

Has anyone tried using Teflon sleeves when setting up glassware? I remember a web site that claimed using the sleeves avoided having to use grease in the joints. The sleeves were .005" thick (thin!).

[Rhodium]

It works down to ~25 mmHg, but lower than that and the sleeves are leaking in air.

[Mercury]

Yeah, I would expect that, but perhaps they are more suitable for applications under atmospheric conditions, not reduced pressure.

[Bond_DoubleBond]

wash with dh2o after naoh washes.  if swim remembers what he once read correctly, naoh in your dcm/ketone will surely fuck up your ketone.

and you say your fridge compressor pulls 30"?  that thing must be a goddam monster.  what's the make and model of it?

[Just4Fun]

SWIM has a brand new Robinair Cooltech 15600 he bought at our favorite auction site for $199 and it is pulling a 30" vacuum.