WillD

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Reaction scheme:
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Reagents:
  • 4'-Methylpropiophenone (cas 5337-93-9) 5 kg;
  • Сooper(II) oxide (CuO) 2.7 kg;
  • Isopropyl alcohol (IPA) 50 l;
  • Iodine 6.5 kg;
Equipment and glassware:
RbAZqduFBX

  • 100 L Batch reactor, which is equipped with drip funnel, top stirrer, thermometer, temperature control system (cooling) and reflux condenser;
  • Funnel;
  • Several buckets 25 L or more;
  • Barrel 100 L;
  • Beaker 2000 mL;
  • Vacuum source;
  • Scale;
  • Measuring cylinder 1000 mL;
  • Glass rod and spatula;
  • Scoops;
  • Nutsche filter;
  • Rotary evaporator;
  • Shovel;

Synthesis:
1. 4'-Methylpropiophenone 5 kg and IPA 50 l are added into a 100 L batch reactor.
2. Stirrer is turned on.
3. Сooper(II) oxide fine powder 2.7 kg is slowly added to the mixture with a stirring.
4. Iodine (I2) 6.5 kg is added to the mixture with stirring as well.
5. The reaction mixture is heated to 70 °C, then reaction is left for 24 h with a constant stirring and heating.
6. After, the stirrer is turned off. The solution is left to precipitate copper. The heating is continued.
7. 2-Iodo-4'-methylpropiophenone solution is decanted from precipitate through a top of the reactor.
8. The solution is put into a freezer for 24 h.
9. 2-Iodo-4'-methylpropiophenone crystals are filtered through a
nutsche filter, washed with cold IPA on the filter.
10. Filtered solution 2/3 is distilled off in
rotovap, crystallized and washed again.
11. 2-Iodo-4'-methylpropiophenone crystals are
dried under vacuum or on air. Yield is 6.5 kg.

2-Iodo-4'-methylpropiophenone synthesis (cas 236117-38-7)

⚙️
  • Three-necked round bottom flask 2000 mL;
  • Stirrer with heating surface and water bath;
  • Schott funnel and Buchner flask;
  • Beakers;
  • Scale;
  • Measuring cylinder 100 mL;
🛢️
  • 4'-Methylpropiophenone (4-MP; cas 5337-93-9) 100 g;
  • Iodine (I2) 128 g;
  • Isopropyl alcohol (IPA) 1000 mL;
  • Сooper(II) oxide (CuO) 53 g;
(00:50) - Distilled water is poured 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) - Copper oxide (CuO) 53 g is added to Rm through the powder funnel.
⚠️ Copper oxide (CuO) have to be distributed throughout the Rm volume with stirring.

(2:22) - Next, dry Iodine 128 g is added in several portions. Fraction of Iodine does not matter (granular or crystalline).
⚠️ Iodine is dissolved in IPA. Remember that Iodine is a halogen and an exhaust ventilation have to be used in safety reasons.

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

(3:11) - Changes in Rm is observed after 15-20 h from the reaction start. The reaction can be carried out at this temperature regime for a longer time, but not less than 15 hours.

(3:30) - The stirrer is turned off. Copper compounds have to be precipitated in entire solution volume.

(3:38) - Rm is decanted. Copper precipitates are left in the vessel. The precipitate is disposed.

(3:52) - Rm is alcohol solution of 2-Iodo-4'-methylpropiophenone. It is cooled at room temperature, and then put into a freezer for 12 hours.

(4:00) - 2-Iodo-4'-methylpropiophenone is crystallized in a beaker. A suction filter system is prepared and IPA (to wash the crystallized product) is cooled in the freezer.

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

(4:45) - 2-Iodo-4'-methylpropiophenone (cas 236117-38-7) final yield is 130 g.
 
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BHBlueberry

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

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
 

WillD

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CryoThio

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No. There will be problems with purity and yield.

Yes, but the mechanisms of reactions are slightly different.
WillDCan you describe what the reaction with copper bromide would look like?
 

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 ??
 

Katty Korner

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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 ??
Venom2021Anyway to replace the p toluene sulfonic acid.
 

yin-yang

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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
 

mrreese

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@William Dampier could I use 4'-chloropropiophenone instead of 4'-Methylpropiophenone?

sorry about the stupid question but i read both phenones are similar in behavior.
 

hustla

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It is possible to recover Copper (II) Oxide after iodination, wash it and later use again, right? It's a catalyst?
 

w2x3f5

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It is possible to recover Copper (II) Oxide after iodination, wash it and later use again, right? It's a catalyst?
hustlahe binds HI, thereby shifting the equilibrium of the reaction towards the formation of iodopropiophenone
 

Katty Korner

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Beginner question, but is the yield to the methyl cathinone higher with the iodo than the bromo?
 

Zefsaid23

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Hi! Beginner question: could I use propiophenone instead of 4'-Methylpropiophenone to make ephedrone (methcathinone) ?
 

Katty Korner

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Hi! Beginner question: could I use propiophenone instead of 4'-Methylpropiophenone to make ephedrone (methcathinone) ?
Zefsaid23Propiophenone will yield methcathinone, yes. Same steps, afaik, just substitute it, and do the math on moles, etc. But im not a chemist either, just like the subject.
 
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