Riccardo Grigolato…………………….My next video is going to be about the best type of silica gel needed to make Na SG. And how to make (M SG) metal silica gel. Mainly (Na SG) sodium silica gel and all the stages/phases the Na SG can exist as. Well actually stage/phase 0 can not be made with sodium. You would need NaK alloy so it is liquid at room temp. Then in the winter when I open my lab I will try the experiment and if I succeed I will make a video on it. Did I answer you question?
@@jbsc6180 yes thanks, my interest is in the actual reduction, guess I just have to wait. Also the support for the sodium is super important so I'will watch your future videos with attention.
Ricacardo Grigalata……….. If you want to read up on Na SG patents.google.com/patent/US7709410B2/en patents.google.com/patent/US7709410B2/en en.wikipedia.org/wiki/M-SG_reducing_agent www.organic-chemistry.org/namedreactions/bouveault-blanc-reduction.shtm en.wikipedia.org/wiki/Silica_gel#Preparation www.organic-chemistry.org/chemicals/reductions/sodium-na.shtm en.wikipedia.org/wiki/Bouveault-Blanc_reduction
Also I bought a cornelius keg which is a stainless steel vessel that can take 130 psi which is about 8 or 9 atmospheres of pressure. It has outlets so I can connect a hydrogen tank to it and build up the pressure to 130psi and reduce methyl benzoate ester into methanol and benzyl alcohol with the help of some copper chromite catalyst. Methyl benzoate is made from a food preservative and gas line antifreeze and a little drain cleaner. All easily bought. A used cornelius keg is PROBABLY 40 or .$50 and new one is PROBABLY 75 or $100. Does this reaction work...……… YES. Does it give good yields...….. .YES. Will it work at 90C at 130 psi...……..I do NOT know but the only way to know is to try. It may need more heat or pressure for all I know
Home made silica gel (SiO2) has an average pore size of 48 nm. The smallest pore size you should have is 50 nm. So home made sand should be good enough for making NaSG but definitely not perfect. Most but not all kitty litter uses Type C silica gel. Which I believe/guess is 85 to 250 nm which is also good enough. Almost perfect. Although the particle size is a bit bigger than you want but it may work good. But you need to make sure they are using ONLY type C silica gel in the kitty litter you use. The only way to know for sure is by doing experiments
I just bought an Led blue light. Be careful when buying a blue LED cause if it is cheap that most likely means it is a white LED bulb with a blue plastic cover over the white LED bulbs and this is not good for benzyl free radical chlorination. The blue light I bought is mostly 450 to 460 nm blue visible light. $30 / bulb which is cheap for a blue LED bulb like tha
I think the reason for the 15 to 1 ratio for the sodium is because some of the sodium Will react with the alcohols to form sodium methoxide or sodium Ethoxide if ethanol is used
Sean Nye...………….. I like your thinking. Before I saw the mechanism on Wikipedia I actually thought that was how the mechanism went. It made alkoxide and that reacted to make the benzyl alcohol. I understand you want to put extra sodium and alcohol in cause some of the sodium will react with the alcohol to make a sodium alkoxide. But why does the first equation use a 15 to 1 ratio and the second equation only use a 4.5 to 1 ratio??????????????/ Is Na D15 that much better than Na SG? Cause that is really the only difference other than the proton donor. The lower ratio reaction uses isopropanol and the higher ratio reaction uses I think methanol. MY GUESS would be it is the Na D15 sodium is better than the NaSG stage 1 sodium. But I have no clue really. I can only guess. This reaction is DEFINITELY getting done this winter. I am so curious if I can do it and what yield I can get. NEED SODIUM !!!!!!!!!!!!!!!!!! I think that will be the only real hassle. And even if I used stoichiometric amounts I still need 4 MOLES OF SODIUM for every mole of ester. THAT IS A LOT FOR ME !!!!!!!!!!!!!! AAAAAAAHHHHHHHHHH LOL. I might try to see if someone will buy me some on ebay. 100 grams should be enough to figure it all out. Crap if I do 1/4 mole reactions I need 1 mole of sodium, Damn a 100 grams would only let me do 4 experiments. That is a lot of experiments to figure it all out. OH well. Never made any large amounts of metals. Guess its time to learn. Maybe it is not as bad as I think. Hey did you see nurd rage finally figured out how to extract LARGER amounts of sodium out of the sodium aggregate you make with NaOH and Mg metal.
I Think that the reason for the 4.5 to 1 ratio using NA-D15 boils down to a few factors like the choice of hexane instead of THF as the reaction solvent and the limited solubility of isopropyl alcohol in hexane along with the lower reaction temperature... And I think ISOpropyl alcohol is a better proton donor than Ethel alcohol or methyl alcohol for this specific reaction... I'm still having a hard time finding out exactly what the dispersion agent is In Na-D 15 but I will keep looking I am curious to find out what exactly is going on ....
I would also suggest taking all of your glassware that you will use during the reaction and putting them in your oven overnight to drive off as much water as possible and right before you assemble your reaction apparatus heating them gently with a propane torch to drive off any more water that will be present that's what you are supposed to do before you do a Grignard reaction and I believe this technique will help improve your yield. Because it seems kind of water sensitive I would also recommend storing all of your liquid reagents on molecular sieves right up until you are ready to pour them into your reaction set up. and I don't know if this will work I still have to look into this a bit more but possibly putting molecular sieves into the reaction mixture itself May help sequester any water that may be present or that is generated during the reaction.
And yes I did see the entire series of videos that nerd rage made it about making sodium metal from sodium hydroxide and magnesium shavings I thought it was a very good project and he made excellent progress. Now the home chemist has a very easy and pretty efficient way to generate metallic sodium. It shouldn't be too hard for you to buy sodium from eBay if you live in the United States you can get sodium lithium potassium and even cesium relatively easily from eBay and pretty cheap
Sean Nye..........I did think that about the alcohol. I was guessing the isopropanol was a better proton donor. I REALLY thought the solvent really did NOT play that big of a factor. But I like what your saying about the limited solubility of isopropanol in hexane. NEVER THOUGHT OF THAT. Sounds great though. I mean they are dripping in the alcohol so they probably do not want a lot of alcohol in there at one time and the limited solubility would help with that. I was going to use hexane any way but was just doing it on a hunch. Now I have a REAL reason to use the hexane instead of ether. Yeah if you find anything out about the Na D15 let me know cause I am not even trying to look in to it at this time. To much work I have at my job now. Also I did put some computer addresses in the description of this video and I think 2 are on how to make Na SG and tells about the different phases/stages if you want to check them out
chem player is back on youtube .just in case you didn't know check this out ruclips.net/channel/UCsJHe4uMbquncMpe1PiLa2A and www.bitchute.com/channel/2vWmMgSEZ2jf/
very nice video, will you make a second video showing all this reactions?
Riccardo Grigolato…………………….My next video is going to be about the best type of silica gel needed to make Na SG. And how to make (M SG) metal silica gel. Mainly (Na SG) sodium silica gel and all the stages/phases the Na SG can exist as. Well actually stage/phase 0 can not be made with sodium. You would need NaK alloy so it is liquid at room temp. Then in the winter when I open my lab I will try the experiment and if I succeed I will make a video on it. Did I answer you question?
@@jbsc6180 yes thanks, my interest is in the actual reduction, guess I just have to wait. Also the support for the sodium is super important so I'will watch your future videos with attention.
Ricacardo Grigalata……….. If you want to read up on Na SG patents.google.com/patent/US7709410B2/en patents.google.com/patent/US7709410B2/en
en.wikipedia.org/wiki/M-SG_reducing_agent www.organic-chemistry.org/namedreactions/bouveault-blanc-reduction.shtm en.wikipedia.org/wiki/Silica_gel#Preparation www.organic-chemistry.org/chemicals/reductions/sodium-na.shtm
en.wikipedia.org/wiki/Bouveault-Blanc_reduction
Also I bought a cornelius keg which is a stainless steel vessel that can take 130 psi which is about 8 or 9 atmospheres of pressure. It has outlets so I can connect a hydrogen tank to it and build up the pressure to 130psi and reduce methyl benzoate ester into methanol and benzyl alcohol with the help of some copper chromite catalyst. Methyl benzoate is made from a food preservative and gas line antifreeze and a little drain cleaner. All easily bought. A used cornelius keg is PROBABLY 40 or .$50 and new one is PROBABLY 75 or $100. Does this reaction work...……… YES. Does it give good yields...….. .YES. Will it work at 90C at 130 psi...……..I do NOT know but the only way to know is to try. It may need more heat or pressure for all I know
Home made silica gel (SiO2) has an average pore size of 48 nm. The smallest pore size you should have is 50 nm. So home made sand should be good enough for making NaSG but definitely not perfect. Most but not all kitty litter uses Type C silica gel. Which I believe/guess is 85 to 250 nm which is also good enough. Almost perfect. Although the particle size is a bit bigger than you want but it may work good. But you need to make sure they are using ONLY type C silica gel in the kitty litter you use. The only way to know for sure is by doing experiments
I just bought an Led blue light. Be careful when buying a blue LED cause if it is cheap that most likely means it is a white LED bulb with a blue plastic cover over the white LED bulbs and this is not good for benzyl free radical chlorination. The blue light I bought is mostly 450 to 460 nm blue visible light. $30 / bulb which is cheap for a blue LED bulb like tha
I think the reason for the 15 to 1 ratio for the sodium is because some of the sodium Will react with the alcohols to form sodium methoxide or sodium Ethoxide if ethanol is used
Sean Nye...………….. I like your thinking. Before I saw the mechanism on Wikipedia I actually thought that was how the mechanism went. It made alkoxide and that reacted to make the benzyl alcohol. I understand you want to put extra sodium and alcohol in cause some of the sodium will react with the alcohol to make a sodium alkoxide. But why does the first equation use a 15 to 1 ratio and the second equation only use a 4.5 to 1 ratio??????????????/ Is Na D15 that much better than Na SG? Cause that is really the only difference other than the proton donor. The lower ratio reaction uses isopropanol and the higher ratio reaction uses I think methanol. MY GUESS would be it is the Na D15 sodium is better than the NaSG stage 1 sodium. But I have no clue really. I can only guess. This reaction is DEFINITELY getting done this winter. I am so curious if I can do it and what yield I can get. NEED SODIUM !!!!!!!!!!!!!!!!!! I think that will be the only real hassle. And even if I used stoichiometric amounts I still need 4 MOLES OF SODIUM for every mole of ester. THAT IS A LOT FOR ME !!!!!!!!!!!!!! AAAAAAAHHHHHHHHHH LOL. I might try to see if someone will buy me some on ebay. 100 grams should be enough to figure it all out. Crap if I do 1/4 mole reactions I need 1 mole of sodium, Damn a 100 grams would only let me do 4 experiments. That is a lot of experiments to figure it all out. OH well. Never made any large amounts of metals. Guess its time to learn. Maybe it is not as bad as I think. Hey did you see nurd rage finally figured out how to extract LARGER amounts of sodium out of the sodium aggregate you make with NaOH and Mg metal.
I Think that the reason for the 4.5 to 1 ratio using NA-D15 boils down to a few factors like the choice of hexane instead of THF as the reaction solvent and the limited solubility of isopropyl alcohol in hexane along with the lower reaction temperature... And I think ISOpropyl alcohol is a better proton donor than Ethel alcohol or methyl alcohol for this specific reaction... I'm still having a hard time finding out exactly what the dispersion agent is In Na-D 15 but I will keep looking I am curious to find out what exactly is going on ....
I would also suggest taking all of your glassware that you will use during the reaction and putting them in your oven overnight to drive off as much water as possible and right before you assemble your reaction apparatus heating them gently with a propane torch to drive off any more water that will be present that's what you are supposed to do before you do a Grignard reaction and I believe this technique will help improve your yield. Because it seems kind of water sensitive I would also recommend storing all of your liquid reagents on molecular sieves right up until you are ready to pour them into your reaction set up. and I don't know if this will work I still have to look into this a bit more but possibly putting molecular sieves into the reaction mixture itself May help sequester any water that may be present or that is generated during the reaction.
And yes I did see the entire series of videos that nerd rage made it about making sodium metal from sodium hydroxide and magnesium shavings I thought it was a very good project and he made excellent progress. Now the home chemist has a very easy and pretty efficient way to generate metallic sodium. It shouldn't be too hard for you to buy sodium from eBay if you live in the United States you can get sodium lithium potassium and even cesium relatively easily from eBay and pretty cheap
Sean Nye..........I did think that about the alcohol. I was guessing the isopropanol was a better proton donor. I REALLY thought the solvent really did NOT play that big of a factor. But I like what your saying about the limited solubility of isopropanol in hexane. NEVER THOUGHT OF THAT. Sounds great though. I mean they are dripping in the alcohol so they probably do not want a lot of alcohol in there at one time and the limited solubility would help with that. I was going to use hexane any way but was just doing it on a hunch. Now I have a REAL reason to use the hexane instead of ether. Yeah if you find anything out about the Na D15 let me know cause I am not even trying to look in to it at this time. To much work I have at my job now. Also I did put some computer addresses in the description of this video and I think 2 are on how to make Na SG and tells about the different phases/stages if you want to check them out
chem player is back on youtube .just in case you didn't know check this out ruclips.net/channel/UCsJHe4uMbquncMpe1PiLa2A and www.bitchute.com/channel/2vWmMgSEZ2jf/