If there is, say, 0.2% water in there, then adding acetic anhydride and distilling it all seems pretty painful. Its 500 mL I think.
I guess I could add a little acetic anhydride then just distill a small amount of acetic acid as I need it.
I wonder if I could do the trick where I reflux it with the setup is rbf under open addition funnel containing of sieves with a condenser on top of that. The reaction to adsorb most of the water is pretty fast, but aldol condensation on the sieves takes some time. After letting it reflux under the sieves for a while, I can then reduce the temperature and run a reaction in the rbf on the bottom.
If there is, say, 0.2% water in there, then adding acetic anhydride and distilling it all seems pretty painful. Its 500 mL I think.
I guess I could add a little acetic anhydride then just distill a small amount of acetic acid as I need it.
I wonder if I could do the trick where I reflux it with the setup is rbf under open addition funnel containing of sieves with a condenser on top of that. The reaction to adsorb most of the water is pretty fast, but aldol condensation on the sieves takes some time. After letting it reflux under the sieves for a while, I can then reduce the temperature and run a reaction in the rbf on the bottom.
acetic acid BP 118, acetic anhydride BP 139 - so disitillation will leave the acetic anhydride behind.
Mol sieves are often problematic for carbonyls - not good for acetone for example, will slowly catalyze aldol reactions. I can see something similar for the acetic acid and especially for any acetic acid solutions with acetic anhydride!
acetic acid BP 118, acetic anhydride BP 139 - so disitillation will leave the acetic anhydride behind.
Mol sieves are often problematic for carbonyls - not good for acetone for example, will slowly catalyze aldol reactions. I can see something similar for the acetic acid and especially for any acetic acid solutions with acetic anhydride!
1). You add a little amount of acetic anhydride and wait a little bit until crystallization below 15oC. If not, you add a little more acetic anhydride. Don’t worry about a little excess of acetic anhydride because it will soon be transformed to glacial acetic acid, as being highly hygroscopic. 2). Yes, molecular sieves are aluminum silicate and alkali/alkali earth aluminosilicate complex salts and thus, they can react even, with weak acids.
1). You add a little amount of acetic anhydride and wait a little bit until crystallization below 15oC. If not, you add a little more acetic anhydride. Don’t worry about a little excess of acetic anhydride because it will soon be transformed to glacial acetic acid, as being highly hygroscopic. 2). Yes, molecular sieves are aluminum silicate and alkali/alkali earth aluminosilicate complex salts and thus, they can react even, with weak acids.
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I guess I could add a little acetic anhydride then just distill a small amount of acetic acid as I need it.
I wonder if I could do the trick where I reflux it with the setup is rbf under open addition funnel containing of sieves with a condenser on top of that. The reaction to adsorb most of the water is pretty fast, but aldol condensation on the sieves takes some time. After letting it reflux under the sieves for a while, I can then reduce the temperature and run a reaction in the rbf on the bottom.
I guess I could add a little acetic anhydride then just distill a small amount of acetic acid as I need it.
I wonder if I could do the trick where I reflux it with the setup is rbf under open addition funnel containing of sieves with a condenser on top of that. The reaction to adsorb most of the water is pretty fast, but aldol condensation on the sieves takes some time. After letting it reflux under the sieves for a while, I can then reduce the temperature and run a reaction in the rbf on the bottom.
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Mol sieves are often problematic for carbonyls - not good for acetone for example, will slowly catalyze aldol reactions. I can see something similar for the acetic acid and especially for any acetic acid solutions with acetic anhydride!
Mol sieves are often problematic for carbonyls - not good for acetone for example, will slowly catalyze aldol reactions. I can see something similar for the acetic acid and especially for any acetic acid solutions with acetic anhydride!
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Don’t worry about a little excess of acetic anhydride because it will soon be transformed to glacial acetic acid, as being highly hygroscopic.
2). Yes, molecular sieves are aluminum silicate and alkali/alkali earth aluminosilicate complex salts and thus, they can react even, with weak acids.
Don’t worry about a little excess of acetic anhydride because it will soon be transformed to glacial acetic acid, as being highly hygroscopic.
2). Yes, molecular sieves are aluminum silicate and alkali/alkali earth aluminosilicate complex salts and thus, they can react even, with weak acids.
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I will if I have to.
I will if I have to.
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