Pseudoephedrine from cold medicine, extraction method.

[hacke8]

Hello fellow chemists. Today I brought a cold medicine (capsule) containing pseudoephedrine hydrochloride. There are 8 capsules in a box. Each capsule contains 90 mg of pseudoephedrine, totaling 0.72 grams. It is very cheap at US$1.5. Here are its ingredients: Each capsule contains 90 mg of pseudoephedrine hydrochloride. mg, chlorpheniramine maleate (chlorpheniramine) 4 mg. The auxiliary materials are: starch, sucrose, hydroxypropyl methylcellulose, ethyl cellulose polymer, Opadry yellow dry spray material, Opadry pink dry spray material. How can I maximize extraction?
My own extraction steps are: open the capsule - soak in 99% ethanol - suction filtration - evaporate the filtrate to the extract - add cold water to the extract (glue will appear) - suction filtration - adjust the filtrate to alkali PH12+ and then extract, (xylene ) Dry the extract - after drying, pass in hydrogen chloride gas (the pH reaches acidity) - filter with suction to obtain white pseudoephedrine hydrochloride powder. But I tried several extractions and only got very little pseudoephedrine. Is there any way to increase the yield?

 

[hacke8]

@G.Patton
Sir, please help me find out the problem. The yield is too low.

 

[G.Patton]

http://bbzzzsvqcrqtki6umym6itiixfhni37ybtt7mkbjyxn2pgllzxf2qgyd.onion/threads/ephedrine-extraction-from-pills-methods.2443/

Hi, try the second method with toluene instead of xylene.
how much did you get?

 

[hacke8]

Hi, sir, I got a 40% yield according to my method. In the second way, I can't buy naphtha.

 

[G.Patton]

How much grams? Naphta can be substituted by PE or white spirit or hexane.

 

[hacke8]

I extracted 6.1 grams from 14.4 grams of pseudoephedrine pills. But the purity is very good, white and flawless. There is no need for recrystallization, and it can be reacted directly.

 

[G.Patton]

What is a weight one tablet?

 

[hacke8]

sorry sir. Translation software always makes us wrong, I mean I extracted 6.1 grams from a pill that contained 14.4 grams of pseudoephedrine. The yield is 40%. Although I don't use it, the quality is very good, as white as snow, and it can be used directly for the next step. I can't get naphtha and methyl ethyl ketone, they are pipe products, in method 2, PE cannot be used. My existing solvents are: ethanol, DCM, PE, xylene, distilled water, sulfuric acid, hydrochloric acid, hypophosphorous acid, glacial acetic acid, acetone and some other reagents (sodium hydroxide-sodium chloride-sodium carbonate-sodium sulfate)

 

[hacke8]

I'm glad to hear from you. Thank you, sir. I bought 20 boxes of medication, each containing 8 pills, each containing 90 milligrams of pseudoephedrine hydrochloride. The total content is 14.4 grams of pseudoephedrine hydrochloride, and I extracted 6.1 grams. Detailed extraction process: 1. I soaked the pill in anhydrous ethanol for 1 hour (room temperature/stirring). 2. Then filter and rinse the solid filter cake with new ethanol (the ethanol extract is very viscous and difficult to filter, so I used an 800 mesh filter). 3. Evaporate the filtered ethanol extract to a diluted state. 4. Adding ice water (distilled water) while stirring will result in gel like substances. 5. Filter out the gel and rinse the colloid with new ethanol. 6. Alkalize the filtrate with sodium hydroxide solution to pH 12 and let it stand for 30 minutes (using cold 20% sodium hydroxide). 7. Pour into a separating funnel and extract with xylene three times. 8. Combine xylene and dry (using anhydrous sodium sulfate). 9. Filter (clean anhydrous sodium sulfate with new xylene). 10. Then, dry hydrogen chloride gas (sulfuric acid+sodium chloride) is introduced to form a white precipitate (stop ventilation after there is no more precipitate). 11. Then filter and dry at room temperature for 1 day. 6.1 grams of pseudoephedrine hydrochloride after constant weight. My question: 1. Do you need to twist the soaking pills into powder (the pills inside the capsules are very small). Do soaking pills require heating? 3. What solvent can dissolve hydroxypropyl methyl cellulose, ethyl cellulose polymer, opal yellow dry spray, opal pink dry spray, and remove them in advance.

 

[G.Patton]

I don't know for sure about form of your pills. Try to do ground them into a powder and see difference.
You can try a little to speed up dissolution procedure

 

[hacke8]

Yes, sir, I'm going to grind the pill into powder on the original basis and heat the ethanol during the soaking process.

 

[hacke8]

It is a capsule-type drug. I take the capsule apart and keep the small particles in the capsule, which shows that it is covered with Obadai dry powder, pink and light yellow.