edo
02-13-04 18:36
       Swim is doing a MM benzo wacker(1/2 ...
(Rated as: UTFSE!) 		    
 
 
 
    pickler
(Greenhorn)
02-15-04 03:07
No 488814
       Yup, your on the right track.     

Yup, your on the right track.
I went into the business for the money, and the art grew out of it.-Charlie Chaplin

 
 
 
 
    edo
02-15-04 03:23
       thx pickler, I did use TFSE
(Rated as: insignificant) 		    
 
 
 
    edo
(Stranger)
02-15-04 04:35
No 488824
       Shit! Swim doing mm wacker and forgot to dry...     

Shit! Swim doing mm wacker and forgot to dry his ketone with 50g magnesium sulfate and he already distilled. Is that a big deal? 		 
 
 
 
    wyndowlicker
02-15-04 08:03
       HEy now,
(Rated as: insignificant) 		    
 
 
 
    Rhodium
(Chief Bee)
02-15-04 09:43
No 488862
       Distilling without drying     

Distilling without drying works, but may cause troublesome bumping in the process, and the water will be sucked into your pump, reducing its efficiency.
The Hive - Clandestine Chemists Without Borders 		 
 
 
 
    edo
(Stranger)
02-19-04 20:07
No 489882
       shit, Swim should of washed with H2O a few...     

shit,
 Swim should of washed with H2O a few times after the NaOH wash. the whole thing turned in a big black chardfrown(polymerized) Swim smashed the flask to save magnetic stirr bar.  
Swim still learning the hard way 		 
 
 
 
    amine
(Hive Bee)
02-19-04 20:42
No 489889
       did you try removing the gunky mess with ...     

did you try removing the gunky mess with hotwater before attempting to smash the flask? generally hot/boiling water will get the tar out.
;) 		 
 
 
 
    Bond_DoubleBond
(Newbee)
02-19-04 22:45
No 489904
       refluxing some dcm in the flask works ...     

refluxing some dcm in the flask works extremely well to remove that tar.  or if you wanna be lazy, put some dcm in the flask and run some hot water over the flask until the dcm starts boiling and swirl it around a bit.  and if you don't wanna use your solvent dcm, you can get dcm containing (>80%) paint and adhesive removers from just about any hardware store for pretty cheap.

once your washing techniques start to improve, you won't get much of that tarry shit.  swim considers h2o washes to be essential after washing with any acid or alkaline solution.  and don't just stop with one water wash.  perform h2o washes until the ph of the aqueous phase is near neutral. 		 
 
 
 
    edo
(Stranger)
02-20-04 15:35
No 490062
       Swim knew to was with H2O after NaOH wash but...     

Swim knew to was with H2O after NaOH wash but swim was tired as shit and forgot. Swim will remember the hot water/DCM to remove tar.(Hopefully never again)
Swim shouldn't have rushed but Swim had success first time making ketone and was eager to repeat it.
thx