Hello,
I stumbled across this synthesis manual and I have a few questions to it.
Though it is in german, maybe you can translate it...
Synthese: In einem 10-ml-Zentrifugenglas werden 28,5 mg Morphin, 29,4 mg N,N-(Dimethylamino)-pyridin, 1 ml Dichlormethan (DCM) und 100 µ l Essigsäureanhydrid vorgelegt. Das Gemisch bleibt nun 5 bis 6 min stehen. Nach Ablauf der Zeit wird das Gemisch mit 2 ml Wasser versetzt und in einem Scheiderichter mit 10 ml Dichlormethan ausgeschüttelt. Das Wasser wird abgetrennt und die organische Phase mit wasserfreiem Natriumsulfat getrocknet. Nach dem Verdampfen des Lösungsmittels bleibt Heroin zurück.
1. If 2ml water was added to 100 yl Acetanhydrid and 1ml Chloroform wouldnt that make the rest of the unreacted Acetanhydrid dilute in the water and react to Acetic Acid?
1b) wouldnt the acetic acid then extract a part of the heroin base into the acidic water phase?
2. If you have as much 4-DMAP in the mixture (which is better soluble in DCM than in water, and it is a solid material, wouldnt after evaporating the DCM there be not only Heroin but more 4DMAP left over?
I think those are 2 big Question marks to this synthesis, but I have not a deep knowledge to chemistry...
I Also have some questions not related to the synthesis but to a purification process or crystallisation process.
3. What is the "Morphine acid tartrate" and the "neutral salt of it" Isnt there just Morphine-tartrate and Morphine-base? What should be the sour salt of Morphine tartrate (if the tartrate is the neutral salt?)
4. If from a mixture of 1-butanol and toluol morphine is extracted with 1% tartric acid water solution, wouldnt then also a part of the 1-butanol also dissolve in the water and later, when the morphine tartrate is cut out again with ammonia, wouldnt then the morphine base not go into solution with the partial 1-butanol that solved in the water? Also it couldnt be dried out from the water then other way around.
5. (very important basic question) Would it also be possible to extract a base into the salt from a pure organic phase like DCM+Morphine-base with a watery acidic solution? Or would the acid never reach the Morphine-base, as it is completely separately from the water (with the acid).
Maybe someone can help me out! I would be extremely thankful if some expert chemist would school me about my (maybe dumb) questions.
Thank you already,
Darksmoke.
I stumbled across this synthesis manual and I have a few questions to it.
Though it is in german, maybe you can translate it...
Synthese: In einem 10-ml-Zentrifugenglas werden 28,5 mg Morphin, 29,4 mg N,N-(Dimethylamino)-pyridin, 1 ml Dichlormethan (DCM) und 100 µ l Essigsäureanhydrid vorgelegt. Das Gemisch bleibt nun 5 bis 6 min stehen. Nach Ablauf der Zeit wird das Gemisch mit 2 ml Wasser versetzt und in einem Scheiderichter mit 10 ml Dichlormethan ausgeschüttelt. Das Wasser wird abgetrennt und die organische Phase mit wasserfreiem Natriumsulfat getrocknet. Nach dem Verdampfen des Lösungsmittels bleibt Heroin zurück.
1. If 2ml water was added to 100 yl Acetanhydrid and 1ml Chloroform wouldnt that make the rest of the unreacted Acetanhydrid dilute in the water and react to Acetic Acid?
1b) wouldnt the acetic acid then extract a part of the heroin base into the acidic water phase?
2. If you have as much 4-DMAP in the mixture (which is better soluble in DCM than in water, and it is a solid material, wouldnt after evaporating the DCM there be not only Heroin but more 4DMAP left over?
I think those are 2 big Question marks to this synthesis, but I have not a deep knowledge to chemistry...
I Also have some questions not related to the synthesis but to a purification process or crystallisation process.
3. What is the "Morphine acid tartrate" and the "neutral salt of it" Isnt there just Morphine-tartrate and Morphine-base? What should be the sour salt of Morphine tartrate (if the tartrate is the neutral salt?)
4. If from a mixture of 1-butanol and toluol morphine is extracted with 1% tartric acid water solution, wouldnt then also a part of the 1-butanol also dissolve in the water and later, when the morphine tartrate is cut out again with ammonia, wouldnt then the morphine base not go into solution with the partial 1-butanol that solved in the water? Also it couldnt be dried out from the water then other way around.
5. (very important basic question) Would it also be possible to extract a base into the salt from a pure organic phase like DCM+Morphine-base with a watery acidic solution? Or would the acid never reach the Morphine-base, as it is completely separately from the water (with the acid).
Maybe someone can help me out! I would be extremely thankful if some expert chemist would school me about my (maybe dumb) questions.
Thank you already,
Darksmoke.
