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.
