I have attempted this with a number of different solvents
It would be helpful to explain what you have tried already (and the results of these attempts).
I have tried extracting by bubbling HCl gas through the EtOAc solution, and recrystallizing with dry IPA however I almost always end up with a fine white powder, extremely low yield (<20%). I have also used EtOH for recrystallization with similar results.
I tried a liquid/liquid extraction adjusting the pH until it was around 5.2 using 1000ml of distilled water and HCl solution but separated out into three layers: A heavy oil looking layer which sunk to the bottom of the beaker, water layer (reasonably clear) and what looked like the EtOAc on the top with some of the base suspended in it. The top layer resembled a dish and was not flat across the bottom which I found puzzling.
I have attempted this with a number of different solvents
It would be helpful to explain what you have tried already (and the results of these attempts).
I have tried extracting by bubbling HCl gas through the EtOAc solution, and recrystallizing with dry IPA however I almost always end up with a fine white powder, extremely low yield (<20%). I have also used EtOH for recrystallization with similar results.
I tried a liquid/liquid extraction adjusting the pH until it was around 5.2 using 1000ml of distilled water and HCl solution but separated out into three layers: A heavy oil looking layer which sunk to the bottom of the beaker, water layer (reasonably clear) and what looked like the EtOAc on the top with some of the base suspended in it. The top layer resembled a dish and was not flat across the bottom which I found puzzling.
I'm not really sure what you mean by an "organic ketone base"? Can you please elaborate?
Sorry, the compound is a ketone, but it is an alkaloid. The part I'm struggling with is the reaction from the base to the acid salt, I had worded it wrong.
I'm not really sure what you mean by an "organic ketone base"? Can you please elaborate?
Sorry, the compound is a ketone, but it is an alkaloid. The part I'm struggling with is the reaction from the base to the acid salt, I had worded it wrong.
It would be helpful to explain what you have tried already (and the results of these attempts).
It would be helpful to explain what you have tried already (and the results of these attempts).
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HBr, MsOH?
HBr, MsOH?
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I have tried extracting by bubbling HCl gas through the EtOAc solution, and recrystallizing with dry IPA however I almost always end up with a fine white powder, extremely low yield (<20%). I have also used EtOH for recrystallization with similar results.
I tried a liquid/liquid extraction adjusting the pH until it was around 5.2 using 1000ml of distilled water and HCl solution but separated out into three layers: A heavy oil looking layer which sunk to the bottom of the beaker, water layer (reasonably clear) and what looked like the EtOAc on the top with some of the base suspended in it. The top layer resembled a dish and was not flat across the bottom which I found puzzling.
I have tried extracting by bubbling HCl gas through the EtOAc solution, and recrystallizing with dry IPA however I almost always end up with a fine white powder, extremely low yield (<20%). I have also used EtOH for recrystallization with similar results.
I tried a liquid/liquid extraction adjusting the pH until it was around 5.2 using 1000ml of distilled water and HCl solution but separated out into three layers: A heavy oil looking layer which sunk to the bottom of the beaker, water layer (reasonably clear) and what looked like the EtOAc on the top with some of the base suspended in it. The top layer resembled a dish and was not flat across the bottom which I found puzzling.
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Sorry, the compound is a ketone, but it is an alkaloid. The part I'm struggling with is the reaction from the base to the acid salt, I had worded it wrong.
Sorry, the compound is a ketone, but it is an alkaloid. The part I'm struggling with is the reaction from the base to the acid salt, I had worded it wrong.
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VOTE