Synthesis of 1-Dimethylamino 2Chloropropane
2.25 ml of 1-dimethylamino-2-propanol with 5 ml of chloroform solvent Inside the two-necked flask Poured under argon gas And place the system inside the ice bath until its temperature reaches zero degrees Celsius Then dilute 2 ml of thionyl chloride with 1 ml of chloroform
And then with the Pasteur pipette little by little into the system add It is placed at room temperature for 30 minutes, so that during this time the liquid inside the flask becomes sediment and heated again for 30 minutes at a temperature of 61 degrees Celsius until the deposit becomes liquid During boiling, SO2 and HCl gas is released.And then they continue heating until the substance inside the flask form sediment again. The precipitate formed is 1-dimethylamino-2-chloropropane hydrochloride . Then wash it several times with ether to remove impurities and then crystallized with ethanol, which has a melting point
It is 191 degrees Celsius.
And then water was poured on the crystal to dissolve completely.
And then 20% NaOH is added to it,
that the desired substance is insoluble in NaOH and becomes two-phase,
that phase Above is the desired substance dissolved in ether . It is separated by a decanter funnel. and then to ether solution NaSO4 was added . After removing the solvent, the raw material is obtained as an oil.
Synthesis of 2-2-dimethylaminovaleronitril
Mix 1 gram of diphenylacetonitrile with 1.5 ml of dimethylformamide (DMF) in a two-necked flask. under gas Argon . After one hour, she added 0.4 grams of sodium hydroxide (NaOH) inside the flask . Then he poured oil into the bathroom . Set the temperature to 78 degrees Celsius . And according to the article, it turns dark purple .Then 0.8 ml of 1-dimethylamino-2-chloropropane was added . Then the reaction mixture at temp 78°C for 24 hours under argon gas . Then the obtained product is diluted with some water and extracted three times by toluene. She separated the desired substance dissolved in toluene with a funnel-decanter .
Wash the material containing toluene once more with saturated sodium chloride.
Then in Toluene NaSO4 is poured to dry and After removing the solvent, a yellow crystalline material is formed . A yellow crystalline material is formed which has
It is an impurity and has two isomers and a small amount of the main substance. The yellow material was washed several times with cold hexane . One of the isomers is thus separated, its melting point is 69°C.
And the other isomer is dissolved in hexane due to heating and becomes a crystal at room temperature.
In this way, the crude product obtained from warm hexane was crystallized and 2,2-diphenyl-4-dimethylaminovaleronitrile
Its melting point is 90 degrees Celsius.
Methadone
A solution of ethyl magnesium bromide (prepared with 0.5 g of magnesium and 1.5 ml of ethyl bromide) in 8 ml
Tetrahydrofuran (THF) was prepared dry. 0.5 g of 2,2-diphenyl-4-dimethylaminovaleronitrile in 1 ml From hot xylene without water During 15 minutes, he injects the glass syringe into the system that prepared Greenyard
has done . Then we wait until the temperature reaches 78 degrees Celsius . After mixing for 5.30 hours It is heated under reflux. Then the solution containing 0.8 ml of hydrochloric acid (37.5%) and 0.8 ml of water is added to the hot reaction mixture for 10 minutes, and then the hot mixture is removed and mixed with 0.2.
18% HCl is washed and after cooling the acidic solution, methadone hydrochloride crystals come. Pour the boiling solution into 2.8 ml of water containing 0.02 g of boiling activated charcoal. They filter the remaining activated carbon and rinse with a small amount of hot water. A solution of 0.08 g of sodium hydroxide in 0.2 ml of water was added to the following filtered mixture and the methadone was crystallized under the influence of cold. which is collected and boiled in some methanol and the solution is filtered to remove some of the suspended solid. And then it is diluted with water until it becomes a little cloudy, and after cooling the solution, white crystals of methadone are formed. It can be collected and washed with a small amount of methanol and dried under vacuum. Dried methadone weighs 0.5 g and therefore melts at 76 °C (product yield 91.9).
drying solvents
Chloroform: First, they shake the water 5 to 6 times with half the volume until about one percent of ethanol is added to it. Chloroform must be removed to stabilize. Then dry over anhydrous calcium chloride for at least 24 hours and then distilled in the presence of P4O10. Dry chloroform is unstable and is a toxic and dangerous gas when exposed to light Produces phosgene. Therefore, dry chloroform should be kept away from light.
Tetrahydrofuran (THF) was first kept for some time on sodium tape to dry as much as possible. when If dry THF is required, the THF containing the sodium strip is refluxed under argon gas and to that amount
Benzophenone is added and the reflux process continues until the color of THF turns purple. Then distill the required amount of THF
done and examined. The reason for the purple color of the solution when THF dries is related to the formation
Radical-anion [ph-Co-ph] by sodium band and benzophenone in the absence of water molecules.
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2.25 ml of 1-dimethylamino-2-propanol with 5 ml of chloroform solvent Inside the two-necked flask Poured under argon gas And place the system inside the ice bath until its temperature reaches zero degrees Celsius Then dilute 2 ml of thionyl chloride with 1 ml of chloroform
And then with the Pasteur pipette little by little into the system add It is placed at room temperature for 30 minutes, so that during this time the liquid inside the flask becomes sediment and heated again for 30 minutes at a temperature of 61 degrees Celsius until the deposit becomes liquid During boiling, SO2 and HCl gas is released.And then they continue heating until the substance inside the flask form sediment again. The precipitate formed is 1-dimethylamino-2-chloropropane hydrochloride . Then wash it several times with ether to remove impurities and then crystallized with ethanol, which has a melting point
It is 191 degrees Celsius.
And then water was poured on the crystal to dissolve completely.
And then 20% NaOH is added to it,
that the desired substance is insoluble in NaOH and becomes two-phase,
that phase Above is the desired substance dissolved in ether . It is separated by a decanter funnel. and then to ether solution NaSO4 was added . After removing the solvent, the raw material is obtained as an oil.
Synthesis of 2-2-dimethylaminovaleronitril
Mix 1 gram of diphenylacetonitrile with 1.5 ml of dimethylformamide (DMF) in a two-necked flask. under gas Argon . After one hour, she added 0.4 grams of sodium hydroxide (NaOH) inside the flask . Then he poured oil into the bathroom . Set the temperature to 78 degrees Celsius . And according to the article, it turns dark purple .Then 0.8 ml of 1-dimethylamino-2-chloropropane was added . Then the reaction mixture at temp 78°C for 24 hours under argon gas . Then the obtained product is diluted with some water and extracted three times by toluene. She separated the desired substance dissolved in toluene with a funnel-decanter .
Wash the material containing toluene once more with saturated sodium chloride.
Then in Toluene NaSO4 is poured to dry and After removing the solvent, a yellow crystalline material is formed . A yellow crystalline material is formed which has
It is an impurity and has two isomers and a small amount of the main substance. The yellow material was washed several times with cold hexane . One of the isomers is thus separated, its melting point is 69°C.
And the other isomer is dissolved in hexane due to heating and becomes a crystal at room temperature.
In this way, the crude product obtained from warm hexane was crystallized and 2,2-diphenyl-4-dimethylaminovaleronitrile
Its melting point is 90 degrees Celsius.
Methadone
A solution of ethyl magnesium bromide (prepared with 0.5 g of magnesium and 1.5 ml of ethyl bromide) in 8 ml
Tetrahydrofuran (THF) was prepared dry. 0.5 g of 2,2-diphenyl-4-dimethylaminovaleronitrile in 1 ml From hot xylene without water During 15 minutes, he injects the glass syringe into the system that prepared Greenyard
has done . Then we wait until the temperature reaches 78 degrees Celsius . After mixing for 5.30 hours It is heated under reflux. Then the solution containing 0.8 ml of hydrochloric acid (37.5%) and 0.8 ml of water is added to the hot reaction mixture for 10 minutes, and then the hot mixture is removed and mixed with 0.2.
18% HCl is washed and after cooling the acidic solution, methadone hydrochloride crystals come. Pour the boiling solution into 2.8 ml of water containing 0.02 g of boiling activated charcoal. They filter the remaining activated carbon and rinse with a small amount of hot water. A solution of 0.08 g of sodium hydroxide in 0.2 ml of water was added to the following filtered mixture and the methadone was crystallized under the influence of cold. which is collected and boiled in some methanol and the solution is filtered to remove some of the suspended solid. And then it is diluted with water until it becomes a little cloudy, and after cooling the solution, white crystals of methadone are formed. It can be collected and washed with a small amount of methanol and dried under vacuum. Dried methadone weighs 0.5 g and therefore melts at 76 °C (product yield 91.9).
drying solvents
Chloroform: First, they shake the water 5 to 6 times with half the volume until about one percent of ethanol is added to it. Chloroform must be removed to stabilize. Then dry over anhydrous calcium chloride for at least 24 hours and then distilled in the presence of P4O10. Dry chloroform is unstable and is a toxic and dangerous gas when exposed to light Produces phosgene. Therefore, dry chloroform should be kept away from light.
Tetrahydrofuran (THF) was first kept for some time on sodium tape to dry as much as possible. when If dry THF is required, the THF containing the sodium strip is refluxed under argon gas and to that amount
Benzophenone is added and the reflux process continues until the color of THF turns purple. Then distill the required amount of THF
done and examined. The reason for the purple color of the solution when THF dries is related to the formation
Radical-anion [ph-Co-ph] by sodium band and benzophenone in the absence of water molecules.
Friends, I found this method and shared with you how to do this procedure? What tools do we need?
I translated this article by Translite, if you have any doubts about the wording, ask me and I will clear it up
