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All 4 posts Subject: 2c-b oxone/kbr reaction so far Please login to post Down

Vaaguh
(Stranger)
04-14-03 20:21
No 426688
      2c-b oxone/kbr reaction so far

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.

Bandil
(Hive Bee)
04-14-03 20:57
No 426691
      I'd say success...

Hi!

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
Bandil

Cops are not there to help you, they're there to bust you.

Vaaguh
(Stranger)
04-15-03 08:51
No 426890
      remainings

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

Vaaguh
(Stranger)
04-15-03 23:05
No 427070
      no success

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.

Hippler

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	All 4 posts		Subject: 2c-b oxone/kbr reaction so far		Please login to post		Down


		Vaaguh (Stranger) 04-14-03 20:21 No 426688				2c-b oxone/kbr reaction so far
						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.



		Bandil (Hive Bee) 04-14-03 20:57 No 426691				I'd say success...
						Hi! 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 Bandil Cops are not there to help you, they're there to bust you.



		Vaaguh (Stranger) 04-15-03 08:51 No 426890				remainings
						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



		Vaaguh (Stranger) 04-15-03 23:05 No 427070				no success
						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. Hippler

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