Methylamine to ephedrine

Methylamine to ephedrine

The invention belongs to the field of medicine and chemical industry, and particularly relates to a preparation method of an ephedrine or pseudoephedrine and an intermediate of ephedrine or pseudoephedrine. Ephedra is a wild plant that has been used for sweating and asthma in Chinese medicine for thousands of years. InJapanese scholar Chang Changyi first separated the mixture of active ingredients from the plant of Ephedra, and its main component was ephedrine.

InMerck Pharmaceuticals isolated pure ephedrine and pseudoephedrine from European ephedra plants. InFreudenberg andBrewster et al. Although both compounds can now be produced by synthetic methods, China still harvests 30, tons of ephedra plants every year, extracting extracts for internal use and exporting.

Such huge consumption has seriously damaged the vegetation in the northwest, which is one of the causes of sandstorms.

In the field of Western medicine treatment, the two are widely used, and the demand is increasing year by year. Ephedrine is used as an adrenergic agonist in hospitals. It has the function of contracting blood vessels and relaxing the respiratory bronchus.

methylamine to ephedrine

It can be used to prevent blood pressure drop, treat nasal congestion, relieve bronchial asthma and allergic urticaria. Pseudoephedrine can be used to relieve mucous membrane congestion in the upper respiratory tract, and to breathe smoothly, so that it is widely used for the adjuvant treatment of colds and colds.

There are several different routes for the synthesis of these two drugs. The typical public reports include the following documents:.

The routes reported in these documents are not applicable to large-scale production in industry, which involves factors such as production costs, labor protection, and environmental protection. The other small part is not suitable for the domestic reagent supply and production equipment.

At present, the general production process at home and abroad is as shown in the following formula. The whole preparation process consists of six steps:. Reports of such chemical reactions can be found in the following journals and patent documents:.

The above synthetic process has the following defects, which cannot meet the technical requirements, safety requirements and environmental protection requirements of modern industrial production:.

First, phosphorous acid is formed in the first step reaction. The presence of large amounts of phosphorus-containing wastewater has created environmental pressures. Secondly, the second step of the Friedel-Craft reaction for the preparation of propiophenone has been reported in the papers J. Socand patent document US 4, respectively.

The yields were After the reaction was completed, the reaction mixture needed to be purified, and a considerable portion of the product was lost in complicated post-treatment and purification operations, such as multiple extractions of diethyl ether, positive and negative washing of water, and expensive Product adsorption during the drying of anhydrous magnesium sulfate and vaporization of the product during vacuum distillation.

The crude product can only be used in the third step after being distilled. In addition, the third step uses expensive bromine, which is a highly volatile liquid and is highly corrosive and often has accidents during transfer, storage and application. Since the bromination reaction uses only one bromine atom and the other bromine atom becomes hydrogen bromide HBr gas, the efficiency is lost, that is, the utilization of bromine is only one-half.

When the concentration of bromine in the localized portion of the reaction is too high or the agitation is poor and the temperature in the local region is too high, the ratio of this by-product rises.The sale of ephedrine, one of the precursors of methamphetamine, is strictly controlled and monitored in various countries to prevent the production of illicit methamphetamine.

There are three kinds of production scheme for ephedrine manufacture, and it is very useful for precursor control to investigate the origin of ephedrine used for the synthesis of illicit methamphetamine. The various origins of ephedrine biosynthetic, semisynthetic, or synthetic could be discriminated clearly by using these values. By the repeated distillation of methylamine in our laboratory, we confirmed that this could be due to isotope separation during distillation for the purification of methylamine used for ephedrine synthesis.

The values for ephedrine used as the precursor were well-correlated with those for methamphetamine synthesized from it. This drug characterization analysis should be useful to illuminate the origin of the precursors used for clandestine methamphetamine and to trace the diversion of medicinal ephedrine for illicit manufacture of methamphetamine.

Isotope ratio analyses at natural abundance levels have been used to establish the environmental source or the geographic origin of various biological and nonbiological materials. Commercial ephedrine is produced by a extraction from ephedra plant, namely biosynthesis; b fully chemical synthesis; and c semisynthesis, as shown in Figure 1. Originally, ephedrine was commonly produced from ephedra plant, but recently, large amounts have been produced by synthesis or semisynthesis.

On the other hand, illicit ephedrine is still generally thought to be produced from ephedra plants. Figure 1 Production schemes of ephedrine: a bromination of propiophenone followed by amination, b fermentation of sugar followed by amination, and c extraction from ephedra plant.

The abuse of amphetamine-type stimulants ATS is an increasing problem. In Asia, including Japan, the abuse of methamphetamine itself is the most serious problem.

Trade in precursors of methamphetamine is strictly controlled and monitored in various countries, since methamphetamine can easily be clandestinely manufactured from its precursors.

To prevent the production of illicit methamphetamine, it is important not only to control and monitor the trade in ephedrine, but also to evaluate the origin of ephedrine used as a precursor of seized methamphetamine by scientific analyses. It is possible to identify the precursor or the method of synthesis of methamphetamine by analyzing impurities in methamphetamine. Chemically, no differences are observed among ephedrine samples produced by different methods.

Furthermore, the isotope ratio of biosynthetic ephedrine will be different depending upon the environmental conditions during growth of the ephedra plants. Thirteen ephedrine hydrochloride samples were used.

Four of them, purchased from Fujiyakuhin Saitama, JapanMaruishi Pharmaceutical Osaka, Japan and Dainippon Pharmaceutical Osaka, Japanwere medicines produced by bromination of propiophenone followed by amination 18 or by extraction from ephedra plants. Three other samples were produced by extraction from ephedra plants, and the rest were produced by fermentation of sugar followed by amination, namely semisynthesis.

Twenty-one illicit methamphetamine samples seized in Japan were also used. Methylamine hydrochloride was purchased from Sigma-Aldrich MO. Figure 2 Synthetic pathways of methamphetamine from ephedrine in this study.

The gases were passed through a copper reactor to reduce NO x to N 2. H 2 O was trapped with Mg ClO 4 2. The stable isotope ratios are expressed relative to the conventional standards, that is, Peedee Belemite for carbon and atmospheric N 2 for nitrogen.

The value is defined according to the following equation:. Each sample was measured five times. The precisions routinely obtained were 0. The resulting free base was distilled by heating.This is a subreddit for Clandestine Chemistry.

We do not condone breaking any laws in your area, but are more than happy for you to share your dreams with us. BatchPurifier - file metadata cleaner for windows. Meth Synthetic Routes self. Are there two main routes that clandestine labs use to make meth, 1 phenylpropanone or 2 pseudoephedrine?

Also, is there no way to make enantiomerically pure meth by starting with P2P since P2P is not stereospecific? Does this mean you must start with pseudoephedrine S chiral center on the carbon containing the amino group ultimately leading to dextromethampetamine rather than any levo to obtain dexromethamphetamine or are there a few things I'm missing here?

Mainly I'm concerned with the probable routes the cartel chemists use to make it. I'd like to believe the pseudo route, however, I thought that in itself was difficult to get ahold of, not necessarily the reagents like methylamine they can get from overseas in China.

Thanks for any info you guys have on this subject or a better subreddit for it.

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There are many ways to produce meth; the two you mentioned are the most popular. Ephedrine already has the nitrogen group attached. In fact, ephedrine is exactly like meth except it has a pesky oxygen group attached making it less lipophilic and precluding it from crossing the blood-brain barrier.

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Sending two electrons to that oxygen group is all that's necessary to cleave it, reducing ephedrine to methamphetamine. Oh and generally the amount of d- or l-isomer that comes from pseudo is dependent on the enantiomeric purity of the starting precursor.

I've heard this is why brand name cold medicine produced better meth than the generics. As to enantiomers. Biker gangs in California produced this during the 60s and 70s. It's heavy on the body load portion, but make no mistake about it: it's powerful.

One can use an acid that exhibits chirality to separate the mixture. There are ways of converting the l-isomer to d as I understand, but it's tedious and low-yielding and pretty much prohibitively expensive for most clandestine operations. Finally, to the Mexican Cartel routes: your guess is probably as good as mine.

Methylamine

The DEA reports shit. They're often either just plain wrong, or they're intentionally disseminating bad information. AFAIK there is no way to convert l-meth into d-meth.

If there were a way to turn it to honey there's no way the DEA would let sales go unregulated. That would take absolutely pure reagents, atmosphere, solvents Just not possible. There is absolutely no difference between generic pseudoephedrine and name brand, other than the fact that name brand Sudafed contains a shitload of povidone and the generics don't.

Besides that, the molecule is the same: d-pseudoephedrine HCl. As for the Mexicans Both ephedrine and pseudoephedrine are globally accounted for. The cartels were smuggling in thousands of metric tons of the shit.

Then Mexico changed its laws, so the smuggling moved to countries more relaxed about it Brazil. I know they aren't using P2P anymore, all the precursors are impossible to get in big enough quantity to run a cartel. I read a world report on precursor diversion recently and it showed that with the increasing difficulty of getting phenylacetic acid the cartels were using regular acetic acid and the results were showing up as impurities in the product.

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If I were to guess I'd say they are doing huge Birch reductions. The fact that it takes a Not economically viable. Ammonia is easy to make and you can get 1g Li batteries at the dollar store, and things being what they are, 0.Methylamine is an organic compound with a formula of CH 3 NH 2.

This colorless gas is a derivative of ammoniabut with one hydrogen atom being replaced by a methyl group.

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It is the simplest primary amine. It is sold as a solution in methanolethanoltetrahydrofuranor wateror as the anhydrous gas in pressurized metal containers. Industrially, methylamine is transported in its anhydrous form in pressurized railcars and tank trailers. It has a strong odor similar to fish. Methylamine is used as a building block for the synthesis of many other commercially available compounds. Methylamine is prepared commercially by the reaction of ammonia with methanol in the presence of an aluminosilicate catalyst.

Dimethylamine and trimethylamine are co-produced; the reaction kinetics and reactant ratios determine the ratio of the three products. The product most favored by the reaction kinetics is trimethylamine. In this way, an estimatedtons were produced in Methylamine was first prepared in by Charles-Adolphe Wurtz via the hydrolysis of methyl isocyanate and related compounds.

In the laboratory, methylamine hydrochloride is readily prepared by various other methods. One method entails treating formaldehyde with ammonium chloride. The colorless hydrochloride salt can be converted to an amine by the addition of a strong base, such as sodium hydroxide NaOH :.

Another method entails reducing nitromethane with zinc and hydrochloric acid. Another method of methylamine production is spontaneous decarboxylation of glycine with a strong base in water.

Methylamine is a good nucleophile as it is an unhindered amine. Its use in organic chemistry is pervasive. Some reactions involving simple reagents include: with phosgene to methyl isocyanatewith carbon disulfide and sodium hydroxide to the sodium methyldithiocarbamate, with chloroform and base to methyl isocyanide and with ethylene oxide to methylethanolamines. Liquid methylamine has solvent properties analogous to those of liquid ammonia.

Representative commercially significant chemicals produced from methylamine include the pharmaceuticals ephedrine and theophyllinethe pesticides carbofurancarbaryland metham sodiumand the solvents N -methylformamide and N -methylpyrrolidone.

The preparation of some surfactants and photographic developers require methylamine as a building block. Methylamine arises as a result of putrefaction and is a substrate for methanogenesis.

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Additionally, methylamine is produced during PADI4 -dependent arginine demethylation. The LD 50 mouse, s. In the United States, methylamine is controlled as a List 1 precursor chemical by the Drug Enforcement Administration [16] due to its use in the illicit production of methamphetamine.

How Meth Works

Its use becomes central to the plot line as an alternative to traditional methamphetamine production techniques that involve pseudoephedrine, a cold medication. From Wikipedia, the free encyclopedia.The production of methamphetamine — and the desire to consume it — is seemingly unstoppable.

When precursor chemicals are brought under tight control in one country, like the United States, production simply moves to another country, such as Mexico. When Mexican authorities clamp down, it moves farther south, or into Europe or Asia.

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Then, the finished product is shipped right back into the very countries that have waged such a battle to eradicate it in the first place. Most meth smuggled into the United States is made in large labs — "superlabs" — in Mexico. There are many small meth labs in operation in the United States, but these mostly serve to feed the habits of the amateur cooks themselves. The production of methamphetamine has been made more difficult by federal regulations, like the Combat Methamphetamine Act ofaimed at controlling the flow of precursor chemicals such as ephedrine and pseudoephedrine found in some cold remediesas well as other necessary components.

Through theft, subterfuge, forgeries, personal connections and sheer willpower, determined cooks are able to collect enough materials to make some home-grown meth. Being determined and being safe are two different things — almost 6 pounds 2.

This fact, however, doesn't stop crystal meth addicts from brewing sloppy batches of fuming, stinking, toxic speed in poorly ventilated environments. Houses used as meth labs are often uninhabitable afterward, and cities and states involved in meth lab busts often don't bother with seizing the property, since nobody in their right mind would purchase it at an auction, even at a steep discount.

Small meth labs can be found in suburban houses, motel rooms, car trunks, in campsites or in the woods. Outdoor operations often result in water contamination and a dying-off of nearby vegetation [source: Snell ]. Large-scale labs are often located inside abandoned barns or warehouses set up specifically for the purpose of factory-line production of methamphetamine.

They aren't necessarily dilapidated properties. They may actually be glistening corporate-style factories that crank out countless pounds of meth per year [source: Matthews ]. Much as a destination can be reached by taking one of several different routes, so too can crystal methamphetamine be produced by a number of different methods, including scary "shake-and-bake" and "one-pot" processes.

All of them, though, involve ephedrine or pseudoephedrine. The entire process can involve as many as 32 different chemicals, but the formula varies by the ingenuity and intelligence of the "chemists" [source: Snell ].

Without getting into an exact recipe, we'll look at how large-scale operations which are more likely to use a methodical and exact approach to their production make crystal meth.

methylamine to ephedrine

This process generally takes about two days' time and can result in hundreds of thousands of methamphetamine doses. Prev NEXT. How to Make Meth. Chemicals and equipment were found in a methamphetamine manufacturing lab following a police raid on Jan. New Zealand Police discovered 75 similar labs across the country. If the ephedrine or pseudoephedrine isn't already in pure powder form, then it must be separated from the tablets of cold medicine that contain it. To do this, the cold medicine tablets are mixed with a solvent and the solution is then filtered and exposed to low temperatures to separate and remove the inert material of the tablet.

The pure pseudoephedrine is then mixed with red phosphorus and hydriodic acid. The red phosphorus is then filtered out and later reusedand the remaining acid is neutralized by adding a lye solution. A substance is added that will bind to the meth, and the liquid meth is then drained out. Hydrogen chloride gas is bubbled through the liquid meth, making it a crystalline hydrochloride salt. This is poured through a filter cloth, and the meth that is left on the filter is then dried. Once dry, the meth is "stepped on" mixed down with inert filler in order to maximize profitsweighed and packaged for shipment or sale.Everything had been considered and taken care of.

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methylamine to ephedrine

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Synthesis of Methamphetamine

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