Vaaguh (Stranger)
04-14-03 22:21
No 426688
      2c-b oxone/kbr reaction so far  Bookmark   

There was 2,5 gram of 2C-H*HCl  dissolved in 20 mL H20. The pH was adjusted to >12 with 20% NaOH and the aqueous layer was extracted with 4x10 mL DCM. The DCM was evaporated to give 2 gram (11mmol) 2C-H freebase, which was dissolved in 10 ml MeOH

There was 1,44 gram  (12mmol) Potassium Bromide in 15 ml MeOH added to the 2c-h freebase solution while being stirred magnetically, in 4 portions there was slowly added 7,46 gram of  Oxone (12mmol ).

After 16 hours of stirring the entire mass was put in the rotovap to distill off the methanol/h2o, however the flask was still slightly warm (reacting) the rotovap was turned on to let it swirl as the reaction might not have gone to completion. 3 Hours later the solution was completely black, does anyone know if reaction has failed perhaps somehow even overoxidized stuff?

currently the solution is being removed from the methanol/h2o and after this a/b extraction will bee the next step to see if there is a success

Below are the pics, 1 from after 16 hours of stirring and 1 that was made 4 hours later.

(Hive Bee)
04-14-03 22:57
No 426691
      I'd say success...  Bookmark   


Well according to my experience it does not take a whole lot of bromine to color anything besides water pitch black-brown. I would definately say that the reaction worked out.

My buck goes on that you have been successfull ;) Please post you results!

Good luck, regards

Cops are not there to help you, they're there to bust you.
04-15-03 10:51
No 426890
      remainings  Bookmark   

The solvents have now been removed and the remainings are a very sticky black oil with solids that are stuck in the flask, later this day there is going to bee added some acetic acid/h2o and it will be washed with dcm, then its being basified, an extraction with dcm will hopefully contain some 2c-b fb. I will keep you guys updated
04-16-03 01:05
No 427070
      no success  Bookmark   

Things ended up as a total mess :( , the reaction shall soon bee repeated.

This time the reaction will not stir for longer then 12 hours.