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What is the best method for carrying out the removal of residual...
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+ Acetonitriles
+ Crystallization
+ Nitriles
+ Rotary evaporator
+ Rid
+ Rotary evaporation
+ Organic chemistry synthesis
+ Ethyl acetate
Posted by
Mike Leslie
What is the best method for carrying out the removal of residual...
Actually i have a doubt ,why the residual solvent cant be acetonitrile, since the b.pt is more for acetonitrile than ethyl acetate. If its ethyl acetate, u can use acetone (volatile) to the mixture and try out your crystallization. Is it only because of the solvent effect? Have you checked the purity of your sample. If minor impurities present, may disturb crystallization.
Actually i have a doubt ,why the residual solvent cant be acetonitrile, since the b.pt is more for acetonitrile than ethyl acetate. If its ethyl acetate, u can use acetone (volatile) to the mixture and try out your crystallization. Is it only because of the solvent effect? Have you checked the purity of your sample. If minor impurities present, may disturb crystallization.
Thank you guys I think I will try to be patient when I use the rotary evaporator and if it doesnt work, I will try adding DCM and work on it again. Thanks a lot.
Thank you guys I think I will try to be patient when I use the rotary evaporator and if it doesnt work, I will try adding DCM and work on it again. Thanks a lot.
Hello Aula: Such problems and difficulties usually happen. As you know both of the solvents you are trying to remove have kind of HIGH boiling point. But still you are using the common method (Vacuum Evaporation using ROTA) to get rid of your solvent. What you need is adjust and control some conditions. Here are some:- 1. You can set your the temperature (of boiling liquid or water) up to 30 Celsius (even up to 40 Celsius) based on your sample's properties. 2. You can decrease the pressure of the ROTA slowly step by step (But keep your aye so that Bumping do not occur). 3. You gat to have patience!!!! Some times it may take hours to get ride of all your solvents. Hope these may help!
Hello Aula: Such problems and difficulties usually happen. As you know both of the solvents you are trying to remove have kind of HIGH boiling point. But still you are using the common method (Vacuum Evaporation using ROTA) to get rid of your solvent. What you need is adjust and control some conditions. Here are some:- 1. You can set your the temperature (of boiling liquid or water) up to 30 Celsius (even up to 40 Celsius) based on your sample's properties. 2. You can decrease the pressure of the ROTA slowly step by step (But keep your aye so that Bumping do not occur). 3. You gat to have patience!!!! Some times it may take hours to get ride of all your solvents. Hope these may help!
Hello. Sometimes when i have this problem i add some DCM and i rotavap again, like 2 or 3 times using some heat (30-40 degrees). In almost cases this works for me. Hope we can help! Good look
Hello. Sometimes when i have this problem i add some DCM and i rotavap again, like 2 or 3 times using some heat (30-40 degrees). In almost cases this works for me. Hope we can help! Good look
The method for carrying out the removal of residual ethyl acetate by vacuum distillation or rotary evaporation. I think there would not be any problem.
The method for carrying out the removal of residual ethyl acetate by vacuum distillation or rotary evaporation. I think there would not be any problem.
Actually i have a doubt ,why the residual solvent cant be acetonitrile, since the b.pt is more for acetonitrile than ethyl acetate. If its ethyl acetate, u can use acetone (volatile) to the mixture and try out your crystallization. Is it only because of the solvent effect? Have you checked the purity of your sample. If minor impurities present, may disturb crystallization.
Actually i have a doubt ,why the residual solvent cant be acetonitrile, since the b.pt is more for acetonitrile than ethyl acetate. If its ethyl acetate, u can use acetone (volatile) to the mixture and try out your crystallization. Is it only because of the solvent effect? Have you checked the purity of your sample. If minor impurities present, may disturb crystallization.
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If the ethyl acetate amount in micro scale you can try withSPME method
If the ethyl acetate amount in micro scale you can try withSPME method
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Thank you guys I think I will try to be patient when I use the rotary evaporator and if it doesnt work, I will try adding DCM and work on it again. Thanks a lot.
Thank you guys I think I will try to be patient when I use the rotary evaporator and if it doesnt work, I will try adding DCM and work on it again. Thanks a lot.
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Hello Aula:
Such problems and difficulties usually happen. As you know both of the solvents you are trying to remove have kind of HIGH boiling point. But still you are using the common method (Vacuum Evaporation using ROTA) to get rid of your solvent. What you need is adjust and control some conditions. Here are some:-
1. You can set your the temperature (of boiling liquid or water) up to 30 Celsius (even up to 40 Celsius) based on your sample's properties.
2. You can decrease the pressure of the ROTA slowly step by step (But keep your aye so that Bumping do not occur).
3. You gat to have patience!!!! Some times it may take hours to get ride of all your solvents.
Hope these may help!
Hello Aula:
Such problems and difficulties usually happen. As you know both of the solvents you are trying to remove have kind of HIGH boiling point. But still you are using the common method (Vacuum Evaporation using ROTA) to get rid of your solvent. What you need is adjust and control some conditions. Here are some:-
1. You can set your the temperature (of boiling liquid or water) up to 30 Celsius (even up to 40 Celsius) based on your sample's properties.
2. You can decrease the pressure of the ROTA slowly step by step (But keep your aye so that Bumping do not occur).
3. You gat to have patience!!!! Some times it may take hours to get ride of all your solvents.
Hope these may help!
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I always use Barbara Bernardim method to remove solvents and it often works.
I always use Barbara Bernardim method to remove solvents and it often works.
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Hello. Sometimes when i have this problem i add some DCM and i rotavap again, like 2 or 3 times using some heat (30-40 degrees). In almost cases this works for me. Hope we can help! Good look
Hello. Sometimes when i have this problem i add some DCM and i rotavap again, like 2 or 3 times using some heat (30-40 degrees). In almost cases this works for me. Hope we can help! Good look
More
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The method for carrying out the removal of residual ethyl acetate by vacuum distillation or rotary evaporation. I think there would not be any problem.
The method for carrying out the removal of residual ethyl acetate by vacuum distillation or rotary evaporation. I think there would not be any problem.
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