Hi all, I received 1 month ago 5 kg of 52190-28-0 from my new supplier @AnnieGalaxy.
The product is brown and it seems similar in smell, texture and appereance like the original 52190-28-0, the problems comes when you try to do the synthesis.
First of all this product is not soluble in DCM or THF, even is not in EtOH as literatures say, thats the first problem.
After i saw this problem i made the melting point proof and the results are the same as the literature say, about 85ºC. This product is only soluble in water.
Knowing the industrial production method of the synthesis of this product i thought that maybe it had impurities like excess of bromine and i washed with sodium thyosulfate 10% solution but it doesnt work.
Finally i tried the synthesis for Bk-M dissolving the product (50gr 52190-28-0) in a saturated water solution/NaHSO3 and after that i add DCM. I wait for layers separation and it seems like the product was in the DCM but when i add methylamine aquous solution the temperature doesnt increase nothing noticing me that there are not methylamination here but even with that indicative i followed the synthesis. After 90 minutes of methylamination i stop the stirring and it produces the layer separation.
I take the organic layer and i add the HCl 37% drop by drop still ph 5.5 and nothing appears after few days.
I tried the synthesis with THF and NMP and nothing happend too.
I want to know if there are more people with the same problem.
I have luck because my new supplier @AnnieGalaxy said me that it was a factory problem before the february chinese holidays and she is going to send me again and for FREE other 5kgs of 52190. I reccomend to work with this supplier, she is very fast answering the questions and giving the quotations.
Thanks to @Acidosis for solving all my doubts with this product checking and this synthesis.
The product is brown and it seems similar in smell, texture and appereance like the original 52190-28-0, the problems comes when you try to do the synthesis.
First of all this product is not soluble in DCM or THF, even is not in EtOH as literatures say, thats the first problem.
After i saw this problem i made the melting point proof and the results are the same as the literature say, about 85ºC. This product is only soluble in water.
Knowing the industrial production method of the synthesis of this product i thought that maybe it had impurities like excess of bromine and i washed with sodium thyosulfate 10% solution but it doesnt work.
Finally i tried the synthesis for Bk-M dissolving the product (50gr 52190-28-0) in a saturated water solution/NaHSO3 and after that i add DCM. I wait for layers separation and it seems like the product was in the DCM but when i add methylamine aquous solution the temperature doesnt increase nothing noticing me that there are not methylamination here but even with that indicative i followed the synthesis. After 90 minutes of methylamination i stop the stirring and it produces the layer separation.
I take the organic layer and i add the HCl 37% drop by drop still ph 5.5 and nothing appears after few days.
I tried the synthesis with THF and NMP and nothing happend too.
I want to know if there are more people with the same problem.
I have luck because my new supplier @AnnieGalaxy said me that it was a factory problem before the february chinese holidays and she is going to send me again and for FREE other 5kgs of 52190. I reccomend to work with this supplier, she is very fast answering the questions and giving the quotations.
Thanks to @Acidosis for solving all my doubts with this product checking and this synthesis.
