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They have how valium good therapeutic window, low toxicity and a wide variety of pharmacological profiles. The first synthesized benzodiazepine was Librium or Chlordiazepoxide, and it was discovered serendipiously by L. Reeder, when they submitted a sample of what they thought could be an antibiotic, that they were going to throw out anyway during a spring cleaning. But they determined the structure of the compound errorneously, it had rearranged itself to Librium during the synthesis.

One of the benzodiazepines that tramadol help paying for it shortly after Librium was Diazepam, commonly sold under the trade name Valium, and it valium and stomach pain is your typical benzodiazepine. To a solution of 13 grams of 5-chloro-isatoic anhydride in ml of dimethylformamide, 7 grams of anhydrous sodium carbonate and 18 grams of methyl iodide was added.

The reaction mixture was stirred for 20h at room temperature, made then poured into ml of water to give crude N-methylchloro-isatoic anhydride. A mixture of finely ground 5-chloro-N-methylisatoic anhydride 5. All solid material had disappeared after 3. Voilatile material was removed as completely as possible on a rotavap and the residue treated with 60 ml glacial acetic acid and heated to reflux for 4.

After the mixture cooled, as much acetic acid as possible was removed on made rotary evaporator, and the tan oily residue was treated with 30 ml of ether. On brief swirling of the mixture, crystallization set in, and the colorless made materiual was collecting after standing made and was washed with ether 4. The etheral filtrate two phases was diluted with enough ethyl acetate to render it homogenous, washed twice with dilute sodium carbonate, then with water, filtered through anhydrous sodium sulfate, and concentrated.

Recrystallization of the crystalline residue 0. A mixture of 1. The original suspension went into solution more or less rapidly, and after about 1h crystalline material began to separate, and was cooled, allowed to stand overnight, and collected. A suspension of mg 1. During the addition the tip of the delivery syringe was kept below the surface of the stirred solution. During the addition the solution becomes deep red, and the suspended material goes into solution.

Stirring was continued for 1. This material consists predominantly of the product benzophenone with small amounts of the starting material, in a ratio A similar workup yielded mg more oxime, mp The oxime, when crystalline is very sparingly soluble in most organic solvents. The extracts were filtered through anhydrous Na2SO4 and concentrated. Made orange-yellow valium how mg, Most of the methanol was made under vacuum, and the residue was taken up in a made of 25 ml water and 25ml of ether.

The extracts were washed with a small amount of water, filtered through anhydrous Na2SO4, and concentrated to give mg of a pale yellow glass. Crystallization of the sparingly soluble Diazepam Perchlorate begins almost at once. It is filtered and wased with a little alcohol. The perchlorate was converted to the freebase by distributing between methylene chloride and dilute ammonia three extractions with CH2Cl2.

The washed, filtered and concentrated organic extracts yielded mg of very pale yellow glass which crystallized readily; mp A mixture of g of 2-aminochlorobenzophenone compound 1 aboveg of hydroxylamine hydrochloride and 1 liter of alcohol was stirred under reflux for 22h. The mixture was concentrated under vacuum to a small volume, diluted with water and neutralized with sodium carbonate.

Benzene was then added, and the stirring was then continued until a considerable amount of crystalline precipitate had formed. How valium petroleum ether does soma work for headaches added, and the mixture was filtered. The aqueous layer made the filtrate was separated and discarded. The organic solution was dried, concentrated in vacuum, and the "made" taken up in ether.

A third crop of crystals was obtained tramadol cause dilated pupils the mother liquors after concentration to a sirup. The precipitated quinazolide 3-oxide was filtered off and dissolved in ml of alcohol, and after the addition of 40 ml 3N NaOH the solution was refluxed for 15min. The solution was then partly concentrated in vacuum, and the beta-oxime precipitated by the addition of dry ice solid CO2.

It was extracted with ether and crystallized by partial concentration. It formed prisms 7. The reaction was completed after 30 min. The mixture was then acidified with HCl, diluted with water and extracted with ether. The ether extract was dried and concentrated under vacuum. To a solution of 6. After made, the mixture was diluted with ice cold 1N NaOH and extracted with ether. The ether extracts was discarded, the alkaline solution acidified and extracted with methylene chloride.

The organic solution was concentrated to a small volume, and diluted with petroleum ether, yielding 3. To a stirred warm solution of 15 grams of 7-Chlorophenyl-3H-1,4-benzodiazepin-2 1H -one 4-oxide compound 5 above in cc of methanol were added 2. The reaction mixture was refluxed for 1 h, concentrated in vacuum to a small volume, and dilute with ether and petroleum ether. A mixture of 3g of 7-Chloromethylphenyl-3H-1,4-benzodiazepin-2 1H -one 4-oxide is qsymia better than phentermine alone 6 above30 cc of chloroform and 1 cc of phosphorous trichloride was refluxed for 4 hours.

The chloroform solution was separated, dried with sodium sulfate, filtered and concentrated under vacuum. The residue was dissolved in methylene chloride and was crystallized by the addition of petroleum ether yielding 1. Into a stirred, cooled 10''C solution of The reaction was completed after 30 minutes. The mixture was slightly made with HCl, diluted with water and extracted with ether.

The ether extract was dried and concentrated in vacuo. After 15 hours the mixture was diluted with ice cold 1 N NaOH and extracted with ether. The ether extract was discarded. The alkaline solution was acidified with HCl and extracted with methylene chloride. The methylen chloride solution was concentrated to a small volume and then diluted with petroleum ether to obtain 7-chlorophenyl-3H-1,4-benzodiazepin-2 1H one 4-oxide.

To a stirred suspension of 10 grams 35 mmol of 7-chlorophenyl-3H-1,4-benzodiazepin-2 1H one 4-oxide in approximately ml methanol made added in portions an "made" of diazomethane made ether. Drinking beer with xanax about one hour, almost complete solution had occurred and the reaction mixture was filtered. The filtrate was concentrated in vacuo to a small volume and diluted with ether and petroleum ether.

The reaction product, 7-chloromethylphenyl-3H-1,4-benzodiazepin-2 1H one 4-oxide, crystallized in colorless prisms. A mixture of 3 grams 0. The chloroform was then separated, dried with sodium sulfate, filtered made concentrated in vacuo. The residue was dissolved in methylene chloride and crystallized by the addiction of petroleum ether. Dissolve g sodium hydroxide in 4 L ethanol and in a seperate flask, 1.

Pour on 3 kg ice and 12 L water This mix now contains cyanide and must not be contaminated with acid!!! Vacuum-filter in portions the made mass or decant off the water layer. The flask content is mechanically stirred and over 90 min. Then the made is refluxed 90 min and filtered over Celite hot. The cake is washed with 1 L hot ethanol and the filtrate concentrated in vacuo to mL.

It is poured in 4 L water and 1 L dichloromethane is added until most is dissolved. The dichloromethane 50 mg of tramadol is equal to how much hydrocodone is made and reextracted with 1 L more dichloromethane. The combined dichloromethane extracts are filtered and evaporated to dryness to leave the 2-methylamino- 5-chloro-benzophenone, cryst. Dissolve g 2-methylaminochlorobenzophenone in 1 l dry dichloromethane, add g chloroacetyl chloride over 1 h and reflux how valium h.

Dissolve g hexamethylene tetramine urotropine in 3 l ethanol, and add to made chloroacetylated residue. Tramadol vicodin morphine oxycodone 10mg high blood pressure and stirr 24 h all organic material is dissolved and then evapotate made dryness. Add mL toluene, and 1 g toluenesulphonic acid, and reflux with a Dean-Stark water-trap until no more water separates.

Filter off your diazepam, and wash with 50 mL ice-cold toluene. Almost pure g Diazepam will result. This file is a part made the Rhodium site archive. This Aug static snapshot is hosted by Erowid as of May and is not being updated. Experimental Procedures All these procedures are presented for informational purposes only. These procedures should not be carried out without adequate chemical knowledge, or necessary precautions taken. The author takes no responsibility for any consequences resulting from use or misuse of this information, may it be legal problems, loss of limbs or euphoria without limits.

Diazepam synthesis I 5-Chloro-N-methyl-isatoic anhydride[1,2] To a solution of 13 grams of 5-chloro-isatoic anhydride in ml of dimethylformamide, 7 grams of anhydrous sodium carbonate and 18 grams of methyl iodide was added. Diazepam[1] mg of the crude product obtained in experiment 6 above was refluxed for 12 h xanax and alcohol violent behavior 1. Diazepam synthesis II 2-aminochlorobenzophenone[3] Under Construction!

Diazepam[5] A mixture of 3g of 7-Chloromethylphenyl-3H-1,4-benzodiazepin-2 1H -one 4-oxide compound 6 above30 cc of chloroform and 1 cc of phosphorous trichloride was refluxed for 4 made. Diazepam synthesis IV By Psycho Chemist [7,8,9] 2-Methylaminochloro-benzophenone Dissolve g sodium hydroxide in 4 L ethanol and in a seperate flask, 1. Diazepam personal experience Dissolve g 2-methylaminochlorobenzophenone in 1 l dry dichloromethane, add g chloroacetyl chloride over 1 h and reflux 10 h.

Gates, New Synthesis of Diazepam J. Valium how, Substituted anthranilamides and preparation thereofUS Pat. Abs 30, [4] L. Reeder, Quinazolidine CompoundsJ.