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All 13 posts Subject: Morphine Extraction Questions? Please login to post Down

beefeater
(Stranger)
11-09-04 22:32
No 540710
      Morphine Extraction Questions?

Hi, I have a couple of questions regarding a patent i found on the extraction and isolation of morphine from opium.Heres a summary.

"In the process, opium is extracted with a basic alcoholic solution. The basic alcoholic solution is filtered and the alcohol removed from the filtrate to leave a residue. The residue is then extracted with
a basic aqueous solution having a pH of at least 11. The basic aqueous solution may be filtered to remove any solid matter remaining after the aqueous extraction step, and then be stirred with a sufficient amount of a salt to avoid emulsion formation. The basic aqueous solution or filtrate is then extracted with benzene or toluene.
Next, adjusting the pH of the basic aqueous filtrate to pH 8.5 to 9.5 allows the morphine to precipitate and be recovered. "

In the statment below he explains that extracting the residue with a basic solution with a pH of atleast 11 turns the free base morphine into it's "anionic" Morphinate. Im kind of confused because the morphine in the opium and dried poppies are kept as the salts of meconic acid (about 90%). After having extracted this morphine with basic alcohol with a pH of 9 is the resulting residue a freebase like sited below? In other extractions not involving Alcohol or caustic alkali
state that when the Morphine Meconate pentahydrate is extracted with slaked lime solution the result is also Morphinate. But with this the Ph is much lower than
11 since youhave to add ammonia to boost up the Ph to 9 to precipitate the morphine. Can someone please help me clear this up, I dont have much knowledge of chemistry and am
confused.

Thanks,

"The resulting residue, which contains the alkaloids, is mixed or extracted with an basic aqueous solution having a pH of atleast 11, preferably an aqueous solution of an alkali hydroxide. This converts the morphine free base present into its anionic (morphinate) form which is soluble in basic solutions at pH values of 11 or above"

beefeater
11-10-04 13:36
      Anyone...anyone....bueller....bueller.............
(Rated as: insignificant)

maj
(Hive Bee)
11-10-04 16:09
No 540839
User Picture       In other extractions not involving Alcohol or...

In other extractions not involving Alcohol or caustic alkali
state that when the Morphine Meconate pentahydrate is extracted with slaked lime solution the result is also Morphinate. But with this the Ph is much lower than

Sure the Ph is lower your extracting with an acidic solution. You can extract with a non-polar solvent or water however until the ph of the solution is 9-9.3 you won't get your precipitants.

I took the one less traveled by,And that has made all the difference.

beefeater
(Stranger)
11-10-04 16:50
No 540842
      Re: Sure the Ph is lower your extracting with...

Sure the Ph is lower your extracting with an acidic solution. You can extract with a non-polar solvent or water however until the ph of the solution is 9-9.3 you won't get your precipitants.

Hydrated lime isnt an acidic solution... Also Morphine is for the most part is insoluble in nonpolar solvents, thats why you use a nonpolar to extract non morphine alkaloids while leaving the morphine in the aqueous solution.

Im wondering is when you mix the morphine meconate with an alkali solution what do you get? Is it a free base?

Nicodem
(Hive Bee)
11-10-04 19:04
No 540878
User Picture       It is said that morphine is amphoteric

Im wondering is when you mix the morphine meconate with an alkali solution what do you get? Is it a free base?

You get the "morphinate", that is the water soluble phenolate form of morphine. Most phenols, since they are slightly acidic, are soluble in water if the pH is high enough. The plain phenol itself has a pKa of about 9 or 10. 2,4,6-trinitrophenol aka picric acid, just as an extreme example, is a relatively strong acid (it has, if I remember corectly, pKa about 1).

Ar-OH + OH^- <=> Ar-O^- + H₂O

So, morphine is soluble in both acidic and strongly basic water solutions, it is however insoluble in the narrow pH range from neutral to just slightly basic solution (pH 7~9).

“The real drug-problem is that we need more and better drugs.” – J. Ott

beefeater
(Stranger)
11-12-04 00:47
No 541127
      A fleeting method on the Alt, drugs, hard...

A fleeting method on the Alt, drugs, hard newsgroup was posted by Jim Hogshire in which the morphine was extracted with Calcium Carbonate and then adding Ammonia to precipitate the Morph. So if you have to add the Ammonia to get the ph up to 9.0 dosent that mean the lime water solution is somewhere between neutral and 9? Or is the ammonia used just too get rid of the calcium salt?

Xaja
(Hive Bee)
11-12-04 10:49
No 541205
User Picture       Maybe

Just from memory, taking pH to 7.8 in aqueus solution then scratching the beaker causes morph to precipitate out, maybe. Not an expert by any means, but think thats right...

**FriedPiper**

I love BUSH! The pussy, not the President!!

Drug_Phreak
(Hive Bee)
11-12-04 13:22
No 541227
      Probably not the info you seek, but on-topic

Morphine is freely soluble in alkaline earth hydroxides. Adding calcium hydroxide/calcium carbonate to the Opium solution only precipitates crap, which is insoluble... leaving the calcium morphinate in solution, which is further precipitated by ammonia to yield Morphine.

Crank is part of this complete breakfast.

tryin
(Newbee)
11-12-04 13:51
No 541233
      Morphine from dried pods

I haven't been able to get the calcium carbonate and ammonium method to work. You can find the explanation of it here Post 43177 (Devil: "Re: opium poppy garden", General Discourse)

Every time the ammonium chloride is added at the end, the product takes on a very ammonia like smell. If anyone has done this method with success please post how you did it.

beefeater
(Stranger)
11-12-04 20:57
No 541276
      "Every time the ammonium chloride is...

"Every time the ammonium chloride is added at the end, the product takes on a very ammonia like smell. If anyone has done this method with success please post how you did it. "

well did you filter the insoluble after you added the Calcium? so what exactly was your problem did the Morphine not precipitate? Methanol or Ethanol is good to add when adding the ammonia to facilitate the crystalization. You left it sit over night to right?

heres a better method using basically the same stuff only with opium and in greater detail.

"Triturate the sample (8 g) with water (30 ml) and calcium hydroxide (2 g) in a mortar. This liberates the alkaloids from their salts, and converts morphine and narcotine into their water soluble calcium salts. Transfer the mixture (grease the lip of the mortar) to a tared flask and make up to exactly 90 g with water. Shake occasionally during half an hour and filter through a dry Buchner funnel into a dry Buchner flask. Transfer exactly 52 ml of the filtrate to a clean dry conical flask, and add ammonium chloride (2 g), ether (25 ml) and 90% ethanol (5 ml). The function of the ammonium chloride is to decompose the calcium salts of the alkaloids.
(RO)2Ca + 2NH4Cl --> 2ROH + 2NH3 + CaCl2

Ether acts as a solvent for narcotine and the ethanol facilitates the crystallization of the morphine which separates from the solution. Cork the flask, shake for 5 minutes and occasionally during half an hour, so that total shaking time is about 15 minutes. Allow to stand overnight. Decant the ethereal solution as completely as possible with a tight plug of cotton wool retaining the crystals in the flask as far as possible. Wash the contents of the flask with a further quantity of ether (10 ml) and decant through the filter. Wash the filter with solvent ether (5 ml) added slowly and in small quantities. Displace the air in the flask gently with air from a bellows to ensure removal of ammonia fumes. Transfer the contents of the funnel back to the flask with water from a wash bottle. Add N/10 [0.1 M] HCl (25 ml), boil gently to remove CO2, and back titrate the excess acid with N/10 [0.1 M] NaOH using methyl red as indicator."

beefeater
(Stranger)
11-12-04 21:12
No 541277
      A book I ordered Arrived yesterday, Its called

A book I ordered Arrived yesterday, Its called Oxy by the notorious Otto Snow. I have to say it cleared up a ton of questions I had about Opiate chemistry. Its a great resourse for people with aspirations of Opiate Production. It is incredibly indepth and offers a broad range of information. Everything from the extraction of Morphine from somniferum and even the extraction of thebaine from The bractaeum variety of poppies also including the synthesis of hydroxycodeinone and Oxycodone from thebaine.
I highly recommend it.

tryin
(Newbee)
11-12-04 21:58
No 541283
      Extraction went wrong

In a nutshell this is what I did and it produced a white powder that smelled very much like ammonia.

http://www.poppies.org/cgi-bin/forum/forum.cgi?az=show_thread&om=319&forum=DCForumID16

beefeater
(Stranger)
11-13-04 01:44
No 541314
      dude that isnt a method of extracting ...

dude that isnt a method of extracting Morphine. Its a way to extract so-called Opium straight from poppy straw without actually tapping the pods.   Basically it is just a smokeable form of "pod putty". If you want The real goods Buy the book I mentioned. You could read the entire poppie.org archive and every patent on the subject and you still wouldnt get what you would from the Book. 25 bucks (from amazon) is definetly worth the info you get.
   If you could'nt allready tell, I'm really psyched from Taking a gander of the book in question.

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	All 13 posts		Subject: Morphine Extraction Questions?		Please login to post		Down


		beefeater (Stranger) 11-09-04 22:32 No 540710				Morphine Extraction Questions?
						Hi, I have a couple of questions regarding a patent i found on the extraction and isolation of morphine from opium.Heres a summary. "In the process, opium is extracted with a basic alcoholic solution. The basic alcoholic solution is filtered and the alcohol removed from the filtrate to leave a residue. The residue is then extracted with a basic aqueous solution having a pH of at least 11. The basic aqueous solution may be filtered to remove any solid matter remaining after the aqueous extraction step, and then be stirred with a sufficient amount of a salt to avoid emulsion formation. The basic aqueous solution or filtrate is then extracted with benzene or toluene. Next, adjusting the pH of the basic aqueous filtrate to pH 8.5 to 9.5 allows the morphine to precipitate and be recovered. " In the statment below he explains that extracting the residue with a basic solution with a pH of atleast 11 turns the free base morphine into it's "anionic" Morphinate. Im kind of confused because the morphine in the opium and dried poppies are kept as the salts of meconic acid (about 90%). After having extracted this morphine with basic alcohol with a pH of 9 is the resulting residue a freebase like sited below? In other extractions not involving Alcohol or caustic alkali state that when the Morphine Meconate pentahydrate is extracted with slaked lime solution the result is also Morphinate. But with this the Ph is much lower than 11 since youhave to add ammonia to boost up the Ph to 9 to precipitate the morphine. Can someone please help me clear this up, I dont have much knowledge of chemistry and am confused. Thanks, "The resulting residue, which contains the alkaloids, is mixed or extracted with an basic aqueous solution having a pH of atleast 11, preferably an aqueous solution of an alkali hydroxide. This converts the morphine free base present into its anionic (morphinate) form which is soluble in basic solutions at pH values of 11 or above"



		beefeater 11-10-04 13:36				Anyone...anyone....bueller....bueller............. (Rated as: insignificant)



		maj (Hive Bee) 11-10-04 16:09 No 540839				In other extractions not involving Alcohol or...
						In other extractions not involving Alcohol or caustic alkali state that when the Morphine Meconate pentahydrate is extracted with slaked lime solution the result is also Morphinate. But with this the Ph is much lower than Sure the Ph is lower your extracting with an acidic solution. You can extract with a non-polar solvent or water however until the ph of the solution is 9-9.3 you won't get your precipitants. I took the one less traveled by,And that has made all the difference.



		beefeater (Stranger) 11-10-04 16:50 No 540842				Re: Sure the Ph is lower your extracting with...
						Sure the Ph is lower your extracting with an acidic solution. You can extract with a non-polar solvent or water however until the ph of the solution is 9-9.3 you won't get your precipitants. Hydrated lime isnt an acidic solution... Also Morphine is for the most part is insoluble in nonpolar solvents, thats why you use a nonpolar to extract non morphine alkaloids while leaving the morphine in the aqueous solution. Im wondering is when you mix the morphine meconate with an alkali solution what do you get? Is it a free base?



		Nicodem (Hive Bee) 11-10-04 19:04 No 540878				It is said that morphine is amphoteric
						Im wondering is when you mix the morphine meconate with an alkali solution what do you get? Is it a free base? You get the "morphinate", that is the water soluble phenolate form of morphine. Most phenols, since they are slightly acidic, are soluble in water if the pH is high enough. The plain phenol itself has a pKa of about 9 or 10. 2,4,6-trinitrophenol aka picric acid, just as an extreme example, is a relatively strong acid (it has, if I remember corectly, pKa about 1). Ar-OH + OH^- <=> Ar-O^- + H₂O So, morphine is soluble in both acidic and strongly basic water solutions, it is however insoluble in the narrow pH range from neutral to just slightly basic solution (pH 7~9). “The real drug-problem is that we need more and better drugs.” – J. Ott



		beefeater (Stranger) 11-12-04 00:47 No 541127				A fleeting method on the Alt, drugs, hard...
						A fleeting method on the Alt, drugs, hard newsgroup was posted by Jim Hogshire in which the morphine was extracted with Calcium Carbonate and then adding Ammonia to precipitate the Morph. So if you have to add the Ammonia to get the ph up to 9.0 dosent that mean the lime water solution is somewhere between neutral and 9? Or is the ammonia used just too get rid of the calcium salt?



		Xaja (Hive Bee) 11-12-04 10:49 No 541205				Maybe
						Just from memory, taking pH to 7.8 in aqueus solution then scratching the beaker causes morph to precipitate out, maybe. Not an expert by any means, but think thats right... FriedPiper I love BUSH! The pussy, not the President!!



		Drug_Phreak (Hive Bee) 11-12-04 13:22 No 541227				Probably not the info you seek, but on-topic
						Morphine is freely soluble in alkaline earth hydroxides. Adding calcium hydroxide/calcium carbonate to the Opium solution only precipitates crap, which is insoluble... leaving the calcium morphinate in solution, which is further precipitated by ammonia to yield Morphine. *Crank is part of this complete breakfast.*



		tryin (Newbee) 11-12-04 13:51 No 541233				Morphine from dried pods
						I haven't been able to get the calcium carbonate and ammonium method to work. You can find the explanation of it here Post 43177 (Devil: "Re: opium poppy garden", General Discourse) Every time the ammonium chloride is added at the end, the product takes on a very ammonia like smell. If anyone has done this method with success please post how you did it.



		beefeater (Stranger) 11-12-04 20:57 No 541276				"Every time the ammonium chloride is...
						"Every time the ammonium chloride is added at the end, the product takes on a very ammonia like smell. If anyone has done this method with success please post how you did it. " well did you filter the insoluble after you added the Calcium? so what exactly was your problem did the Morphine not precipitate? Methanol or Ethanol is good to add when adding the ammonia to facilitate the crystalization. You left it sit over night to right? heres a better method using basically the same stuff only with opium and in greater detail. "Triturate the sample (8 g) with water (30 ml) and calcium hydroxide (2 g) in a mortar. This liberates the alkaloids from their salts, and converts morphine and narcotine into their water soluble calcium salts. Transfer the mixture (grease the lip of the mortar) to a tared flask and make up to exactly 90 g with water. Shake occasionally during half an hour and filter through a dry Buchner funnel into a dry Buchner flask. Transfer exactly 52 ml of the filtrate to a clean dry conical flask, and add ammonium chloride (2 g), ether (25 ml) and 90% ethanol (5 ml). The function of the ammonium chloride is to decompose the calcium salts of the alkaloids. (RO)2Ca + 2NH4Cl --> 2ROH + 2NH3 + CaCl2 Ether acts as a solvent for narcotine and the ethanol facilitates the crystallization of the morphine which separates from the solution. Cork the flask, shake for 5 minutes and occasionally during half an hour, so that total shaking time is about 15 minutes. Allow to stand overnight. Decant the ethereal solution as completely as possible with a tight plug of cotton wool retaining the crystals in the flask as far as possible. Wash the contents of the flask with a further quantity of ether (10 ml) and decant through the filter. Wash the filter with solvent ether (5 ml) added slowly and in small quantities. Displace the air in the flask gently with air from a bellows to ensure removal of ammonia fumes. Transfer the contents of the funnel back to the flask with water from a wash bottle. Add N/10 [0.1 M] HCl (25 ml), boil gently to remove CO2, and back titrate the excess acid with N/10 [0.1 M] NaOH using methyl red as indicator."



		beefeater (Stranger) 11-12-04 21:12 No 541277				A book I ordered Arrived yesterday, Its called
						A book I ordered Arrived yesterday, Its called Oxy by the notorious Otto Snow. I have to say it cleared up a ton of questions I had about Opiate chemistry. Its a great resourse for people with aspirations of Opiate Production. It is incredibly indepth and offers a broad range of information. Everything from the extraction of Morphine from somniferum and even the extraction of thebaine from The bractaeum variety of poppies also including the synthesis of hydroxycodeinone and Oxycodone from thebaine. I highly recommend it.



		tryin (Newbee) 11-12-04 21:58 No 541283				Extraction went wrong
						In a nutshell this is what I did and it produced a white powder that smelled very much like ammonia. http://www.poppies.org/cgi-bin/forum/forum.cgi?az=show_thread&om=319&forum=DCForumID16



		beefeater (Stranger) 11-13-04 01:44 No 541314				dude that isnt a method of extracting ...
						dude that isnt a method of extracting Morphine. Its a way to extract so-called Opium straight from poppy straw without actually tapping the pods. Basically it is just a smokeable form of "pod putty". If you want The real goods Buy the book I mentioned. You could read the entire poppie.org archive and every patent on the subject and you still wouldnt get what you would from the Book. 25 bucks (from amazon) is definetly worth the info you get. If you could'nt allready tell, I'm really psyched from Taking a gander of the book in question.

All 13 posts	End of thread	Top