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Iodination of 4-methylpropiophenone with iodine/cooper(II) oxide (large scale)

William Dampier

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Reaction scheme:
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Reagents:
4-methylpropiophenone 5 kg,
Copper oxide 2,7 kg,
IPA 50 liters,
Iodine 6,5 kg.

Synthesis:
1. Add 5 kg 4-methylpropiophenone and 50 liters of IPA to the reactor.
2. Start stirring.
3. Slowly add 2.7 kg fine powder of copper oxide with stirring.
4. Add 6.5 kg of elementary iodine with stirring.
5. Heat the reaction mixture to 70 *С.
6. Leave when heated and stirring for 24 hours.
7. After this time stop stirring, let fall the copper precipitate. Heating continues.
8. Decanting ketone solution from the precipitate through a top of the reactor.
9. Put a solution in the freezer for 24 hours.
10. Filter the obtained iodoketone crystals through a nutsche-filter, washing with ice IPA on the filter.
11. The filtrate was sent to distillation by evaporating 2/3 mixture, crystallizing and wash again.
12. Dried on vacuum or blowing warm air. Yield: 6.5 kg iodoketone.

2-Iodo-4'-methylpropiophenone synthesis​


⚙️
Three-necked round bottom flask 2000 mL
Stirrer with heating surface and water bath
Reflux condenser
Schott funnel
Single stage vacuum pump
🛢️
4-Methylpropiophenone (4-MP) 100 g
Iodine (I2) 128 g
Isopropyl alcohol (IPA) 1000 mL
Copper oxide (CuO) 53 g
(00:50) - Pour distilled water into the water bath vessel, immerse approximately half of the round bottom flask in water. Better to immerse the flask with reaction mixture (Rm) level in the same level of water in the bath.

(01:07) - Set the heater temperature to 80 °C. The water temperature have to be >60 °C.
Reagents are added to the flask one by one when the water temperature reaches 60 °C.
4-MP (100 g) + IPA (1000 mL) and turn on the stirrer.

(2:00) - Add 53 g copper oxide (CuO) to Rm through the powder funnel.
⚠️ Copper oxide (CuO) have to be distributed throughout the volume of the Rm with stirring.

(2:22) - Next, add dry Iodine 128 g in several portions. Fraction of Iodine does not matter (granular or crystalline).
⚠️ Iodine dissolves in IPA. Remember that Iodine is a halogen, so we have to use exhaust ventilation by safety reason.

(2:46) - Attach Reflux condenser (with cold water flow) to the round bottom flask to condense reaction vapours.
⚠️ An insoluble suspension of CuO and Iodine is observed in Rm, which should uniformly fill all reaction volume by stirring. Otherwise, the reaction will be carried out incorrectly.

(3:11) - After 15-20 hours from the Reflux condenser attaching moment, we observe a changes in Rm. The reaction can be carried out at this temperature regime for longer time, but not less than 15 hours.

(3:30) - Turn off the stirrer. We wait until the entire suspension of copper compounds has precipitated.

(3:38) - Decant Rm, leaving a precipitate in the flask.
The precipitate is disposed.

(3:52) - Rm is alcohol solution of iodoketone, It is cooled at room temperature, and then keep in the freezer for 12 hours.

(4:00) - 2-Iodo-4'-methylpropiophenone is crystallized in a beaker. Prepare the suction filter system and the chilled in the freezer IPA (to wash the filtrate).

(4:27) - 2-Iodo-4'-methylpropiophenone is filtered, washed with chilled IPA, dried to constant weight at room temperature.

(4:45) - Final yield 130 g of 2-Iodo-4'-methylpropiophenone.
 
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BHBlueberry

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Sorry but I have never heard about this - is it a precursor or what?
 

HIGGS BOSSON

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Sorry but I have never heard about this - is it a precursor or what?
It is a precursor for the synthesis of mephedrone, interesting as an analogue for countries where it is banned 4-methyl-alpha-bromopropiophenone.
 

beetlebb

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You can also do a selective bromination using copper (II) bromide
 

ADATA

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Is it possible to lower the IPA or use other methods to lower the capacity
 

Venom2021

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Preparation 2-iodo-4-methylpropiophenone The so-called iodoketone Place in a beaker 4-methylpropiophenone 150ml (148.90g) N-iodosucinimide 270g P-Toulenesulfonic acid monohydrate 228g We cover the glasses with a glass lid not tightly. We put it in the microwave and set it to 700w. We illuminate 3 times for 1 minute with 30-second breaks between sessions. We are waiting for the romance to cool down to temperature. Pour 300 ml of internal water with ice into the water and mix thoroughly. An iodoketone will arise almost immediately We filter on the filter and 2 or 3 more times We wash the water Crystallization 1g of iodoketone add 0.5ml or 0.7ml dcm mixed in a canister and put into the freezer -20 overnight After a night, filter it and then dry it. Yield 210g to 215g of pure iodoketone will me ok ??
 

wannabeechemist

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Is there any difference in yield between I and Br group for amination step?
 

fuckypu

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Bk4 is better to made 4mmc and stronger like jk4
 
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