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G.Patton

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G.Patton sir​

step 8
After pouring crushed ice and NH4CI, what is the concentrated solution?
It means that before the ice water melts
joejoeYou need to reach base pH 12-13, not really matter concentration.
 

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You need to reach base pH 12-13, not really matter concentration.
G.PattonHello Sir, after the sol was made to PH 12-13, a lot of gel appeared and make the extraction by EA almost impossible. Any advice?
 

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Hello Sir, after the sol was made to PH 12-13, a lot of gel appeared and make the extraction by EA almost impossible. Any advice?
neoking8Hi, write please about what step are you talking about, what solution do you mean?
 

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You can substitute decalin by cyclohexane, probably
G.PattonCyclohexane has a boiling point of 81 °C what would mean the thermal rearrangement would need 7 to 10 days at reflux. But then one could use IPA, same bp and it is known to work from literature (7 to 10 days at reflux).

Ethylbenzoate works.
Ethylene Glycol is another solvent which works and of better availability.

The yield is never near to quantitative, actually when using the Ketimine as base yields suffer, for decent yields the HCl salt must be used. It must also be done under strictly anhydrous conditions or yields suck. (the Imine will hydrolyze back to MeNH2, unsurprisingly regarding the rigorous conditions).

The rearrangement is catalyzed by Lewis Acids, MgCl2 And AlCl3 (anhydrous) work well. 0,1 mol equivalent are needed but AlCl3 can also take care of any water still present, the amount used must be adjusted of course, say X g needed to scavenge the water plus 0,1 mol to catalyze the reaction.
The use of AlCl3 reduces the temperature needed to ~130 °C (to take the same time as 180 °C would take un-catalyzed).


Another tip: Stay away from CCl4 the stuff is not just toxic but its mean and hard to get for good reasons. Gladly it is completely unnecessary for brominating the alpha position. The foolproof way to do this is by using CuBr2 what does the job quantitativly and without side-reactions.
For reaction conditions just Google "Bromination with CuBr2" and you will quickly find the standard conditions for this described and those work perfectly well in this case.
 

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Cyclohexane has a boiling point of 81 °C what would mean the thermal rearrangement would need 7 to 10 days at reflux. But then one could use IPA, same bp and it is known to work from literature (7 to 10 days at reflux).

Ethylbenzoate works.
Ethylene Glycol is another solvent which works and of better availability.

The yield is never near to quantitative, actually when using the Ketimine as base yields suffer, for decent yields the HCl salt must be used. It must also be done under strictly anhydrous conditions or yields suck. (the Imine will hydrolyze back to MeNH2, unsurprisingly regarding the rigorous conditions).

The rearrangement is catalyzed by Lewis Acids, MgCl2 And AlCl3 (anhydrous) work well. 0,1 mol equivalent are needed but AlCl3 can also take care of any water still present, the amount used must be adjusted of course, say X g needed to scavenge the water plus 0,1 mol to catalyze the reaction.
The use of AlCl3 reduces the temperature needed to ~130 °C (to take the same time as 180 °C would take un-catalyzed).


Another tip: Stay away from CCl4 the stuff is not just toxic but its mean and hard to get for good reasons. Gladly it is completely unnecessary for brominating the alpha position. The foolproof way to do this is by using CuBr2 what does the job quantitativly and without side-reactions.
For reaction conditions just Google "Bromination with CuBr2" and you will quickly find the standard conditions for this described and those work perfectly well in this case.
OrgUnikumYou mean you must hcl gas the methylketimine before the rearrangement to have decent yields?
 

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Yes, you have to stir this reaction too without heating.

What do you mean?
G.PattonSir,Need to heat to a boil?How long does it take to mix in total?How do know that the reactants have reached saturation after the addition of methylamine?
 

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If this Grignard reaction is not ideal, o-chlorobenzaldehyde can be used, which is easy to react to produce alcohol and then oxidize.
 

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I wonder where I can get these materials.
 

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1-bromocyclopentyl-(o-chlorophenyl)-ketone (CAS 6740-86-9) is commercially available. It is being sold in forms of white powder or brown oil. You mentioned “This bromoketone is unstable and must be used immediately”, if that’s the case then how do they sell it. The solution has a very dark color in most of the photos, is there any point in buying them?
And how about the powder? How can we use the powder?
 

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1-bromocyclopentyl-(o-chlorophenyl)-ketone (CAS 6740-86-9) is commercially available. It is being sold in forms of white powder or brown oil. You mentioned “This bromoketone is unstable and must be used immediately”, if that’s the case then how do they sell it. The solution has a very dark color in most of the photos, is there any point in buying them?
And how about the powder? How can we use the powder?
Dopeyseems no way to find a vendor for 6740.
 

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1-bromocyclopentyl-(o-chlorophenyl)-ketone (CAS 6740-86-9) is commercially available. It is being sold in forms of white powder or brown oil. You mentioned “This bromoketone is unstable and must be used immediately”, if that’s the case then how do they sell it. The solution has a very dark color in most of the photos, is there any point in buying them?
And how about the powder? How can we use the powder?
DopeyHi, it can be stored in a fridge under inert atmosphere. But I'm not sure that it's commercially available.
 

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Hi, it can be stored in a fridge under inert atmosphere. But I'm not sure that it's commercially available.
G.PattonWell, I searched the CAS number on google, and there were a lot of sellers on Echemi, Chemical book, etc. I even saw some sellers on here (bb), you can try.

But if it has to be stored in a fridge and under inert atmosphere then it’s probably not the best option.
 

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after 95 °C for 3-4 hrs,and extracted with 20% HCl. Acidic extract is basified and extracted with DCM. Solvent is removed, giving the product as an oil that DONT crystallizes. Instead, it become extremely sticky brown color oil. and cant not recrystallization from pentane/ether or hexane/ether. any tips?
 

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after 95 °C for 3-4 hrs,and extracted with 20% HCl. Acidic extract is basified and extracted with DCM. Solvent is removed, giving the product as an oil that DONT crystallizes. Instead, it become extremely sticky brown color oil. and cant not recrystallization from pentane/ether or hexane/ether. any tips?
kaka
Instead, it become extremely sticky brown color oil. and cant not recrystallization from pentane/ether or hexane/ether. any tips?
Try to use vacuum chamber for a day. Did you scratched the oil in these solvents by glass rod, tried to place into a fridge?
 
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