Potassium t-butoxide is commercially available as a solution and as a solid, but it is often generated in situ for laboratory use because samples are so sensitive and older samples are often of poor quality. It is prepared by the reaction of dry tert-butyl alcohol with potassium metal.[1] The solid is obtained by evaporating these solutions followed by heating the solid.The solid can be purified by sublimation at 220 °C and 1 mmHg.
Potassium t-butoxide is commercially available as a solution and as a solid, but it is often generated in situ for laboratory use because samples are so sensitive and older samples are often of poor quality. It is prepared by the reaction of dry tert-butyl alcohol with potassium metal.[1] The solid is obtained by evaporating these solutions followed by heating the solid.The solid can be purified by sublimation at 220 °C and 1 mmHg.
It is its own best drying agent, which, unfortunately, is self consuming. Like milk, buy only as much as you need with short-term storage in a dessicator.
It is its own best drying agent, which, unfortunately, is self consuming. Like milk, buy only as much as you need with short-term storage in a dessicator.
As others have suggested, your best bet is to buy a pure sample and make sure you treat it under strictly anhydrous conditions. If you have some material already and you need a pure sample, Carlos above is correct that you can remove t-butanol under vacuum and heat, but that will leave KOH. If that is a problem, one of the tips in this link tells you how to purify small amounts of KOtBu: https://chemtips.wordpress.com/tag/potassium-butoxide/
As others have suggested, your best bet is to buy a pure sample and make sure you treat it under strictly anhydrous conditions. If you have some material already and you need a pure sample, Carlos above is correct that you can remove t-butanol under vacuum and heat, but that will leave KOH. If that is a problem, one of the tips in this link tells you how to purify small amounts of KOtBu: https://chemtips.wordpress.com/tag/potassium-butoxide/
If you're have to keep potassium t-butoxide then use potassium metal in a sure-sealed bottle under dry inert atmosphere (argon or helium). Use only double-ended needles (cannula) with the help of dry argon/helium gas to transfer the exact amount you require.
If you're have to keep potassium t-butoxide then use potassium metal in a sure-sealed bottle under dry inert atmosphere (argon or helium). Use only double-ended needles (cannula) with the help of dry argon/helium gas to transfer the exact amount you require.
Potassium tert-butoxide readily reacts with humidity. You can heat potassium tert-butoxide at ~155 ºC, in vacuum (approx. 2 mmHg), for about 1 h, to evaporate any tert-butanol possibly present as impurity.
Potassium tert-butoxide readily reacts with humidity. You can heat potassium tert-butoxide at ~155 ºC, in vacuum (approx. 2 mmHg), for about 1 h, to evaporate any tert-butanol possibly present as impurity.
tBuOK is well soluble in THF (25g/100g@25oC) but KOH and K2CO3 are not. Dissolve-> filtrate->evaporate to dryness - simple and highly efficient method. tBuOK build complex with tBuOH (!) , but it destroyed below of thermal stability temperature of tBuOK (~ 250°C ) . Vacuum sublimation is good but complex and low productivity method.
tBuOK is well soluble in THF (25g/100g@25oC) but KOH and K2CO3 are not. Dissolve-> filtrate->evaporate to dryness - simple and highly efficient method. tBuOK build complex with tBuOH (!) , but it destroyed below of thermal stability temperature of tBuOK (~ 250°C ) . Vacuum sublimation is good but complex and low productivity method.
Potassium t-butoxide is commercially available as a solution and as a solid, but it is often generated in situ for laboratory use because samples are so sensitive and older samples are often of poor quality. It is prepared by the reaction of dry tert-butyl alcohol with potassium metal.[1] The solid is obtained by evaporating these solutions followed by heating the solid.The solid can be purified by sublimation at 220 °C and 1 mmHg.
Potassium t-butoxide is commercially available as a solution and as a solid, but it is often generated in situ for laboratory use because samples are so sensitive and older samples are often of poor quality. It is prepared by the reaction of dry tert-butyl alcohol with potassium metal.[1] The solid is obtained by evaporating these solutions followed by heating the solid.The solid can be purified by sublimation at 220 °C and 1 mmHg.
Solid KH in paraffin is preferred over KH in mineral oil. It is stable in air and can be used to prepare active t-BuOK as required.
Article Potassium Hydride in Paraffin: A Useful Base for Organic Synthesis
Solid KH in paraffin is preferred over KH in mineral oil. It is stable in air and can be used to prepare active t-BuOK as required.
Article Potassium Hydride in Paraffin: A Useful Base for Organic Synthesis
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Potassium t-butoxide is commercially available as a solution and as a solid, but it is often generated in situ for laboratory use because samples are so sensitive and older samples are often of poor quality. It is prepared by the reaction of dry tert-butyl alcohol with potassium metal.[1] The solid is obtained by evaporating these solutions followed by heating the solid. The solid can be purified by sublimation at 220 °C and 1 mmHg.
Potassium t-butoxide is commercially available as a solution and as a solid, but it is often generated in situ for laboratory use because samples are so sensitive and older samples are often of poor quality. It is prepared by the reaction of dry tert-butyl alcohol with potassium metal.[1] The solid is obtained by evaporating these solutions followed by heating the solid. The solid can be purified by sublimation at 220 °C and 1 mmHg.
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Try to use dessicator with P2O5 and vacuum.
Try to use dessicator with P2O5 and vacuum.
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It is its own best drying agent, which, unfortunately, is self consuming. Like milk, buy only as much as you need with short-term storage in a dessicator.
It is its own best drying agent, which, unfortunately, is self consuming. Like milk, buy only as much as you need with short-term storage in a dessicator.
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Great, thank you all above.
Great, thank you all above.
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As others have suggested, your best bet is to buy a pure sample and make sure you treat it under strictly anhydrous conditions. If you have some material already and you need a pure sample, Carlos above is correct that you can remove t-butanol under vacuum and heat, but that will leave KOH. If that is a problem, one of the tips in this link tells you how to purify small amounts of KOtBu: https://chemtips.wordpress.com/tag/potassium-butoxide/
As others have suggested, your best bet is to buy a pure sample and make sure you treat it under strictly anhydrous conditions. If you have some material already and you need a pure sample, Carlos above is correct that you can remove t-butanol under vacuum and heat, but that will leave KOH. If that is a problem, one of the tips in this link tells you how to purify small amounts of KOtBu: https://chemtips.wordpress.com/tag/potassium-butoxide/
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VOTE
If you're have to keep potassium t-butoxide then use potassium metal in a sure-sealed bottle under dry inert atmosphere (argon or helium). Use only double-ended needles (cannula) with the help of dry argon/helium gas to transfer the exact amount you require.
If you're have to keep potassium t-butoxide then use potassium metal in a sure-sealed bottle under dry inert atmosphere (argon or helium). Use only double-ended needles (cannula) with the help of dry argon/helium gas to transfer the exact amount you require.
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useful
useful
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Why do you need to struggle keeping potassium t-butoxide dry while you can generate it in situ and use it immediately.
Why do you need to struggle keeping potassium t-butoxide dry while you can generate it in situ and use it immediately.
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Potassium tert-butoxide readily reacts with humidity. You can heat potassium tert-butoxide at ~155 ºC, in vacuum (approx. 2 mmHg), for about 1 h, to evaporate any tert-butanol possibly present as impurity.
Potassium tert-butoxide readily reacts with humidity. You can heat potassium tert-butoxide at ~155 ºC, in vacuum (approx. 2 mmHg), for about 1 h, to evaporate any tert-butanol possibly present as impurity.
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tBuOK is well soluble in THF (25g/100g@25oC) but KOH and K2CO3 are not. Dissolve-> filtrate->evaporate to dryness - simple and highly efficient method. tBuOK build complex with tBuOH (!) , but it destroyed below of thermal stability temperature of tBuOK (~ 250°C ) .
Vacuum sublimation is good but complex and low productivity method.
tBuOK is well soluble in THF (25g/100g@25oC) but KOH and K2CO3 are not. Dissolve-> filtrate->evaporate to dryness - simple and highly efficient method. tBuOK build complex with tBuOH (!) , but it destroyed below of thermal stability temperature of tBuOK (~ 250°C ) .
Vacuum sublimation is good but complex and low productivity method.
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VOTE
Potassium t-butoxide is commercially available as a solution and as a solid, but it is often generated in situ for laboratory use because samples are so sensitive and older samples are often of poor quality. It is prepared by the reaction of dry tert-butyl alcohol with potassium metal.[1] The solid is obtained by evaporating these solutions followed by heating the solid. The solid can be purified by sublimation at 220 °C and 1 mmHg.
Potassium t-butoxide is commercially available as a solution and as a solid, but it is often generated in situ for laboratory use because samples are so sensitive and older samples are often of poor quality. It is prepared by the reaction of dry tert-butyl alcohol with potassium metal.[1] The solid is obtained by evaporating these solutions followed by heating the solid. The solid can be purified by sublimation at 220 °C and 1 mmHg.
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VOTE