Амфетамин из фенилаланина

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This is a static mirror of The Vespiary created on June 11, Naf1 Foundress Queen Posts: Phenylalanine to amphetamine or N-methylamphetamine; Historically; There are two routes that have been previously investigated and are documented on Rhodiums website and I am sure everyone reading this has seen. The first method uses Lithium Aluminium Hydride to reduce phenylalanine to phenylalaninol. Then proceeds to protect the amine function, with a carbobenzyloxy Cbz group. Reduction with lithium aluminium hydride affords methamphetamine, all steps proceed with retention of configuration so if one started with D-phenylalanine one would end up with the required S enantiomer. The second route similarily starts by reducing phenylalanine to phenylalaninol this time using lithium borohydride, then protection of the amine functionality with a tert-Butyloxycarbonyl BOC group forming a carbamate. Iodination of the hydroxyl group proceeds, and reduction of the iodo compound with sodium selectride reduces it to its parent hydrocarbon. Triflouroacetic acid removes the BOC protection to leave amphetamine. Also this method proceeds with retention of configuration if you started with D-phenylalanine you would end up with the required S enantiomer. I was hoping to investigate some of the newer more relavent methods that are not the same as above. If anyone wants to add anything please feel free. Phenylacetaldehyde from Phenylalanine Phenylalanine can be treated with nitrous acid to produce phenyllactic acid, nitrous acid is produced from sodium nitrite and any mineral acid. Also alpha methylation of phenylalanine as previously discussed after strecker degradation yields phenylacetone. He was actually quietly telling members via PM to do it, the results were verified via hp chromatography he said. A highly regarded member also wrote this at science madness, adding to the confusion; 'however the alcohol of phenylalanine, phenylalaninol, has been reduced to the alkane Javas comments are true but.. Decreasing the red-p and increasing the reflux to 35 hours will have no effect except the reaction rate will be decreased one third. Ref for iodo; Ref for phenylalaninol reduction Patent no; Ref for bromo; Ring Cleavage of 1-Benzenesulfonylbenzylethylenimine with Hydrogen Bromide http: N-methylation should proceed swiftly at this point! Emiliano Zapata It is better to die on your feet than to live on your knees! German Subordinate Wasp Posts: It is the same premise as all the outstanding patents on making the ester but it is still a little different which makes me wonder where UF pulled it out of his ass from. The patents have continuously adding ethanol while it distills off during the cook. Even the ones that do it under reflux are different. German, there are references for Festers ester reflux. In the patent below example 1 is what you are talking about and comparative example 1 is the reflux but they use a 4 hour reflux instead of Festers 3 hour. Method for preparing amino acid esters EPB1 http: Process for preparing 1-phenylaminopropane http: And there are other examples in that patent that use much more red p and HI! They actually state this in the patent; 'As to the step for the reductive deiodonation of the compound 1-phenylaminoiodopropane , the reaction is carried out preferably at high temperature to produce the desired compound, 1-phenylaminopropane. Suitable reductive dehalogenating agents are Raney nickel and lithium aluminium hydride. Although Hydroiodic acid itself maybe effective as the reductive dehalogenating agent, in this case the reaction is too slow to be practical' And they said that after pushing their reactions out to 35 hours!!! I have refluxed in excess of 48 hours, and adding another 48 would not be the end of the world. But just be aware if you want the complete reduction dehalogenation you are going to have to go stronger than 24 hours. Or at least do some serious experimenting like Java stated. Now I know you cant depend solely on one patent, and trust me I can produce more concerning reduction of primary alcohols with HydroIodic acid. I also dont imagine TLC would provide a clear reading here either, the retention time of the iodo derivative would be too close to descriminate double bubble. Depending on what combination of solvents you used as your eluent, would determine how clear the resolution was. But that being said if it was N-methylated and on testing kept you up for 2 days, there is no disputing that. I have been talking about this alot, because I am somewhat concerned that people will take this easier route and will end up taking iodopropanes instead of the good stuff. I sincerely appreciate your input Java, and was hoping to grill you further on Aziridines in this thread. August 17, , I will start posting some experiments that I have done and been doing that some may find interesting just bear with me. Thank you very much re;Aziridines, I hope you dont mind me laying that procedure out here with the refs and so forth. I have read the WD thread thats why I was interested. Also it lets me catch up with the whole scheme of things and I can start looking into some alternate ring opening reactions. Happyman Subordinate Wasp Posts: I was debating whether to put this under Short Question or this thread so sorry to whoever thinks it belongs under Short Questions. I stumbled upon this at the hive. Seems hard to believe its would of gone unnoticed for over a decade so can someone more qualified then myself shoot it down real fast. The alcohol should be reduced in one step to the alkane, like described in the literature I gave in an earlier post. Other ways to make benzedrine from phenylalaninol usually transform the alcohol to an halide, which is then reduced. But usually the amine needs to be protected for this, adding 2 steps to the sequence. Naf1 on August 17, , As to the step for the reductive deiodonation of the compound 1-phenylaminoiodopropane , the reaction is carried out preferably at high temperature to produce the desired compound, 1-phenylaminopropane. Although Hydroiodic acid itself maybe effective as the reductive dehalogenating agent, in this case the reaction is too slow to be practical' this is because from a mechanistic point of view the aziridine is formed and easily reduced temperatures that high in this type of reduction poses the problem of phosphine gas formation. It is quite disappointing though the number of patents I am coming across lately that simply cant be trusted. It is whether the subsequent reduction of the halo compound can occur in a realistic time frame, as you said I tend to lean strongly towards Javas comments opposed to the patent which historically have been known to be way off the mark. The dehydration of secondary and tertiary alcohols that occurs with hydroiodic acid and red p with ephedrine etc. As they react via a carbocation, and primary alcohols cannot form carbocations so have to react via their halo intermediates. So instead of the fairly expeditious dehydration, a longer more drawn out halogenation followed by reduction of the resulting halopropane results. As you can see from other patents such as; http: Then there is the less common but still encountered method to reduce the resulting halo compound with the nascent hydrogen of reducing agents such as; i. I would have loved if Java or anyone else interested dropped some product into a solution of sodium biphenyl or some such analytical technique; http: Have you noticed the similarity of 1-phenylaminoiodopropane and nitrgen mustard gas. In brief - even traces of 1-phenylaminoiodopropane should be avoided at all cost in the final product!!! I may read some about it. September 25, , I think LAH isnt an option, but what about electrolytic? No chloro or bromo compounds have been found to date for which the reagent is ineffective. The method is particularly adapted to samples containing small amounts of halogen as there is no limit on sample size, although it is equally satisfactory with small samples having a higher halogen content. The method is less suitable for samples containing large amounts of substances with reactive hydrogen such as water, alcohol, etc. The procedure is particularly suitable for routine work because it is simple, rapid, and readily adaptable to multiple determinations. A single determination can be made in 20 minutes once a stock of reagent has been prepared. For routine work eight samples per hour can be run. The low pH will convert the amine group to ammonium ion, which will be untouched by the tosylate. The HCl gas should leave the system. For this purpose 1-phenylaminopropanol-3 sulphate should be reacted directly with tosyl chloride until no more HCl gas is liberated. The reaction should be similar to the rection of nitrating glycerine or methanol, done in highly acidic medium concentrated mixed acids. What do you think, is it possible? Chloramphenicol can obviously be a precursor, but it is having nitro group in p-position making corresponding amphetamine inactive. I wonder if there are any antibiotics analogues of C. Who stuff the banks? Who staff the party ranks? More for Gore or the son of a drug lord? None of the above, fuck it, cut the cord! In the case of secondary amines, 10 mmol of 4a and 50 mmol of 5a were used. For amines with multiple amino functions, 10 mmol of 4a and 50 mmol of 5a were applied per methyl group to be introduced. The vessel was closed and heated to C for 1 h, and to C for 10 min. The reaction mixture was cooled to room temperature. The white, crystalline mass obtained was crushed, and calcium oxide 0. The mixture was stirred vigorously for 30 min, solids were removed by filtration, and the solvent was removed in vacuo to produce the pure amine. Efficient method going from OH to Cl. April 09, ,

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