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Posts by Deprotonater
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2017-06-25 at 8:09 PM UTC in Deleted posts for: Deprotonater
Originally posted by Malice Interesting, I can fast for at least 2 days now pretty easily, without really feeling much hunger. My stomach genuinely hasn't even growled once. 3 days and I would probably start feeling like I should eat, although it would still be manageable.
Occasionally fasting like this actually has considerable benefits. Going to try jogging to the store and see if I notice a distinctly higher mood lift afterward. The various biological shifts that occur from it are likely to augment the effect. Certain noots could amplify this even more, but I don't have any other than NSI-189, which I'm saving for when school starts.
Interesting you mention NSI-189 i'm doing a lot of work on this class of drugs recently.
https://en.wikipedia.org/wiki/Category:Nicotinamides -
2017-06-25 at 6:24 PM UTC in Ephedrine from Propiophenone OTC
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2017-06-25 at 5:27 PM UTC in Methylphenidate + Analogs, total synthesis.I have more on the subject but I can't find anything about it in english for some reason, I will keep digging.
https://www.google.com/patents/US9079928To a solution of protected hydroxyl acid 4 (1 mmol) in DCM (8 mL) was added TEA (2.5 mmol) and the solution was cooled down to 0° C. A solution of 4-nitrophenyl chloroformate (5, 1 mmol) in DCM (2 mL) was added drop-wise at 0° C. After the addition the reaction mixture was slowly brought to room temperature and left overnight. The solvent was evaporated and dried in vacuum to give the carbonate derivative 6. Compound 6 was dissolved in dimethylformamide (DMF) and to the solution were added TEA (3 mmol) and MPH.HCl (1.05 mmol). The mixture was heated for 8 h at 75° C. Solvent was removed under reduced pressure. The residue was dissolved in EtOAc (60 mL) and washed with 5% aq. NaHCO3 (2×40 mL) and brine (1×40 mL). The organic phase was dried over Na2SO4 and evaporated to dryness to give 8, which was purified by preparative HPLC.
In other embodiments, the synthesis of MPH-CO-l-lactate (8b, A=-CH(CH3)—) is as follows:
To a solution of benzyl lactate 4 (A=-CH(CH3)—; 0.39 g, 2 mmol) in DCM (8 mL) was added TEA (0.69 mL, 5 mmol) and the solution was cooled down to 0° C. A solution of 4-nitrophenyl chloroformate 5 (0.436 g, 2.1 mmol) in DCM (3 mL) was added drop-wise at 0° C. Subsequently, the reaction mixture was slowly brought to room temperature and left overnight. The solvent was evaporated in vacuum and dried to give the carbonate derivative 6 (A=-CH(CH3)—). Compound 6 was dissolved in DMF (12 mL) and to the solution were added TEA (0.84 mL, 6 mmol) and MPH.HCl (0.604 g, 2.23 mmol). The mixture was heated for 20 h at 65° C. Solvent was removed under reduced pressure. The residue was dissolved in EtOAc (40 mL) and was washed with 5% aq. NaHCO3 (2×30 mL) and brine (1×30 mL). The organic phase was dried over Na2SO4, evaporated to dryness and purified by preparative HPLC to give 8b (0.62 g). -
2017-06-25 at 5:23 PM UTC in Deleted posts for: DeprotonaterEasiest benzo to make, like making a cake.
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2017-06-25 at 5:01 PM UTC in Ephedrine from Propiophenone OTCI've been dabbling into reduction of propiophenone to the alcohol and looking at the most OTC route possible
TiCl3, NH3 - good yield but to much volume and to many salts. Ticl3 can easily be prepped from Ti powder but it takes a little time. Nice color, deepest blue.
IPA and NaOH in a pressure cooker for few hours or 22h at normal pressure works as stated but reference is incredibly diluted, 25 g in several litres. But its pretty amazing in general.
Hints at the quasi-fact that the MPV-reduction doesnt only work with aluminium isopropoxide (which needs nasty Hg for making it), but that other alkali and earth alkali alkoxides might be able to pull this reaction off, as well, and most important, in a less diluted reaction mix.
That is most promising (except maybe, for what follows at the end of this post) right now and would open MPV-red to the masses.
We should put work into this, Im willing to experiment but others need to check the theory. Magnesium alkoxides would be most amazing, and OTC prep of Na and K alkoxides is supposed to work as well. Maybe even lithium. Could also use that Na-MgO aggregate for making the needed alkoxide.
Unless we would go for a electrochemical reduction method, what would probably work well and maybe even beat the above idea, there are only other reduction methods left, which require "real reduction agents" to be made or aquired.
Dithionite really is a hit, buy it OTC, make yourself by zn and bi sulfite and forget Dioxane or DMF as theyre not necessary. Just look for some older paper using NaOH and dithionite on various ketones in some standard OTC solvent.
Some other rather available reagent along with hydroxide but I forgot which it was. Looked promising an classical.
some notes
https://erowid.org/archive/rhodium/chemistry/ppa.html
https://www.google.com.ar/patents/WO2005100299A1?cl=en -
2017-06-24 at 11:31 PM UTC in P2NP to amine with NaBH4-Copper. One pot, no messing with metals or acids.not important for you just keep scrolling
I was told following:
With vigorous stirring, to 5ml of IPA / 1g of P2NP and 0.4 times volume of H2O in RBF was dumped 6 mol eq. of NaBH4.
Recrystallized P2NP was washed with sodium bisulfite solution, then with and water and it was then added in small portions to the mixture to minimize frothing. No external cooling applied. After all substrate was added and near-colourless solution is obtained, the solution left stirring for 30 minutes. Claisen adapter was fitted to the rbf with reflux setup and addition funnel. With one portion, 10%-mol equivalent (for the nitroalkene) of CuCl2.2H2O dissolved in IPA was added to the solution via the funnel. It was refluxed for 30 minutes. After which the remaining NaBH4 was destroyed by adding about 50% acetic acid untill the fizzing stopped and the solution was fairly acidic. With the claisen adapter still attaced, short path distillation setup was rigged and everything below 100'C was stripped.
Then the solution was made basic dripping strong NaOH solution to the reaction flask and steam distilled. Additional very dilute NaOH solution was added through the addition funnel every now and then. The distillate was then made slightly acidic with H2SO4 and evaporated.
Total yield after recrystallization: 80% mol wise from the P2NP due to very sloppy work
Functional groups can be reduced in the order of ketones > aromatic nitro groups > aliphatic esters > aliphatic nitros > nitriles > olefins. Dunno where to place the halogens though. But basically with methylamine or even nitromethane, you could reduce straight to methamphs as well. How neat is that :)
Notes: use pure IPA (without lubricants and shit like that), maybe ethanol (without mek etc ketones).. and remember to recrystallize the P2NP and/or wash it with sodium bisulfite to get rid of aldehydes. They interfere the reaction. Unfortunately, this reduction does not work with ring halogenations. It will efficiently reduce 4-chloro-2,5-diMeOP2NP to 2,5-DMA though..
The modification is based onISSN: 2231-1963
Please try it yourself and post your results :) I say: fuck the Zn/Al reductions, even though the Al-Cu or even Zn-Cu with formic acid works like a charm (and the yields are quite comparable). But too much work and hassle anyway. Btw, I use 4%-mol of CuCl2.2H2O for the zinc reductions with formic/potassium formate reactions.
http://www.sciencemadness.org/talk/files.php?pid=331291&aid=31340
