TMCP-indole synthesis (UR-144 intermediate, cas 895152-66-6). Large scale.

WillD

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Reaction scheme:
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Equipment and glassware:
  • 50 L Batch reactor, which is equipped with drip funnel, top stirrer, thermometer, temperature control system (cooling) and reflux condenser;
  • Funnel;
  • Several buckets 10 and 20 L;
  • Vacuum source;
  • Laboratory scale (1-2000 g is suitable);
  • Measuring cylinder 1000 mL;
  • Glass rod (big one) and spatula;
  • Nutsche filter;
  • Rotary evaporator;
  • Scoops;

Reagents:
  • Tin (IV) chloride (SnCl4) 2000 ml (cas 7646-78-8);
  • Dichloromethane (CH2Cl2) 15 l;
  • Indole 1000 g (cas 120-72-9);
  • 2,2,3,3-Tetramethylcyclopropanecarbonyl chloride 1371 g (cas 24303-61-5); Supplier
  • Ice distilled water 20 l;
  • Ethyl acetate 15 l;
  • Sodium sulfate Na2SO4 (or MgSO4) anhydrous ~ 2 kg;
Synthesis:
1. Tin (IV) chloride (SnCl4) 2000 ml was added in one portion into a reaction mixture of dichloromethane (CH2Cl2) 15 l with indole 1000 g. Mixture is stirred in a 50 L batch reactor with cooling.
2. Next, reactor cooling is removed and reaction mixture is stirred for 30 min at room temperature. 2,2,3,3-Tetramethylcyclopropanecarbonyl chloride 1371 g (cas 24303-61-5) in small portions and then nitromethane 10 l are added.
3. The mixture is stirred for 2 h at room temperature.
4. Reaction mixture is quenched with ice water 20 l, filtered from inorganic precipitates via
Nutsche filter. Organic substances are extracted with ethyl acetate 15 l.
5. The organic extract is
dried over Na2SO4 (or MgSO4) and concentrated at reduced pressure in rotary evaporator to give the product as a crystals.

UR-144, A-834,735, XLR-11 can be obtained from TMCP-indole intermediate.

The synthesis of this substance is quite complex.
We recommend buying a ready-made precursor, which is quite difficult to find. According to our information, this substance is available in brumer.com
 
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onionexpress

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Where do i find this 2,2,3,3-Tetramethylcyclopropanecarbonyl chloride? Is it a ready synthesis that can i buy or i have to synthesize it ?
 

banister

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I believe there are a few sources left in Poland and the lot. Ask distribution point of contact "Pygmalion".
 

HIGGS BOSSON

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I bought a ready-made 2,2,3,3-Tetramethylcyclopropanecarbonyl chloride in China, but it can also be made from the corresponding acid. But the easiest way would be to find a supplier of TMCP-indole, then the synthesis of UR-144 would be very simple.
 

madmoney69

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Hello.
TMCP-indole, what is CAS no of it?
I think with cas no it would be easier to find, because when I search TMCP-indole it gives me results as it is UR144.
Thank you
 

HIGGS BOSSON

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CAS 895152-66-6
 

onionexpress

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If it’s possible to tell me your supplier I would be thankful .
 

abbadon

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Pygmalion was name of a marketplace vendor, or?
 

abbadon

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Anyone tried this sincerly? I think i should at least try this way. If possible.

Otherwise
i found in the listings section indole from china and CH2Cl2 from india`?
or is Dichloromethane Anhydrous from an european vendor same like CH2Cl2?
Nitromethane also from europe. Correct_?

The other integridents i not found yet. SnCl4 and 2,2,3,3-Tetramethylcyclopropanecarbonyl chloride.
 

WillD

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SnCl4 only anhydrous (it is in the form of a liquid) is required.
can be replaced with 1-naphthoyl chloride, 1-adamantaneacetyl chloride, etc
 

Andreymalikov

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hello tell me please if i use 1-naphtoyl chlorid instead of 2,2,3,3-Tetramethylcyclopropanecarbonyl chloride
The quantities and dosages and Steps of the recipe will remain the same?
Thank you very much
 

Andreymalikov

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hello tell me please if i use 1-naphtoyl chlorid instead of 2,2,3,3-Tetramethylcyclopropanecarbonyl chloride
The quantities and dosages and Steps of the recipe will remain the same?
Thank you very much
 

charmingcho

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Can i see this experimental video?
I'm always fail this experimental.
 

HIGGS BOSSON

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This synthesis is quite difficult. Look for suppliers of ready-made reagent, I know that Brumer sells it.
We are not planning to make a video
 

charmingcho

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I also want to buy intermediate-level substances, but I am not able to try them because it seems illegal to bring them in my country.

Is the reason why this experiment is difficult is because of the crushing of the reaction?
 

WillD

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Then do complete synthesis if you have raw materials. One of the methods here is presented.
 
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