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William D.

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Reaction scheme:
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Equipment and glassware:
Reagents:
RNVFDK2XU5
  • Indole 1000 g, cas: 120-72-9;
  • Dichloromethane (CH2Cl2) 15 liters, cas: 75-09-2;
  • Tin (IV) chloride 2000 ml, cas: 7646-78-8;
  • 1-Naphthoyl chloride 1627 g, cas: 879-18-5;
  • Nitromethane 10 L, cas: 75-52-5;
  • Ethyl acetate 15 L, cas: 141-78-6;
  • Sodium hydroxide 1300 g, cas: 1310-73-2;
  • TBAB 800 g, cas: 1643-19-2;
  • 1-Bromopentane 1500 g, cas: 110-53-2;
  • Distilled water 20 L;
  • Magnesium sulphate (MgSO4);

Step 1. 3-(1-naphthoyl)indole (cas 109555-87-5) from 1-Naphthoyl chloride and Indole.
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1. Tin (IV) chloride (SnCl4) 2000 ml is added in one portion to a indole 1000 g solution in 50 l batch reactor dichloromethane (CH2Cl2) 15 liters with a constant stirring and external cooling by a cold water bath or cold cooling system.
2. Than, reaction mixture is cooled to a room temperature and stirred for 30 min. Next, 1-naphthoyl chloride 1627 g is poured in small portions to the suspension, followed by nitromethane 10 L.
3. The mixture is stirred for 2 h at room temperature.
4. The reaction mixture is quenched with ice water 20 L,
extracted with ethyl acetate 15 L and filtered to remove inorganic precipitates on a nutsche filter.
5. The organic phase is dried over Na2SO4 and MgSO4, filtered from solids and concentrated at reduced pressure to give the 3-(1-naphthoyl)indole (cas 109555-87-5) as a crystals.

Step 2. 1-pentyl-3-(1-naphthoyl)indole (JWH-018) from 3-(1-naphthoyl)indole (cas 109555-87-5).
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1. 3-(1-naphtoyl) indole 2000 g, sodium hydroxide (NaOH) 1300 g, TBAB 800 g are weighed and placed into a 10 L flask.
2. 1-Bromopentane 1500 g and distilled water 3000 ml are poured into the flask.
3. Reaction mixture is stirred until two layers are separated and solid sodium hydroxide is dissolved completely.
4. Sodium hydroxide dissolving is conducted with heat releasing, hence the mixture is self-heated.
5. The flask is put on heating plate and heated with maximum power after two layers are divided and all sodium hydroxide is dissolved.
6. Top stirrer is installed onto the flask. It is necessary to stir the solution well enough so that the layers are mixed in homogeneous mixture.
7. Top stirrer have to work with constant power during reaction.
8. The
mixture is simmered until reaction solution is become milky and homogeneous. It takes 15-30 min.
9. Then, the flask is removed from heating plate and the mixture is separated into two layers.
10. Top layer is needed. The product is crystallized directly in the flask, which makes it difficult to take out. Therefore, procedures are done quickly.
11. Top layer is poured neatly into Pyrex dishes or silicone molds.
12. JWH-018 is left for 24 h in order to crystallization. Silicone molds are taken for convenient handling with JWH-018 product by reason that it is crystallized and taken a form, which it was poured.
13. Crystallized JWH-018 product is taken out and crushed. Then, It is air dried on a paper or a dish in a warm dry well ventilated room (better to use
vacuum desiccator to significantly increase drying speed). Drying procedure depends on amount of JWH-018 product and takes ~48 h. Reaction yield is 3000 g.
 
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a114488

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Can anyone upload a video? About JWH-018 I am a novice
 

William D.

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Can anyone upload a video? About JWH-018 I am a novice
a114488No video, but I can advise in detail on the process here, private message or XMPP. I have enough practical experience on this synthesis.
 

a114488

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Ok sir , I need to ask you a little question ~~~
Do I need a heater to prepare 3-(1-naphthoyl)indole?
Including the reagents you mentioned, if I buy ordinary or inferior reagents, can I continue to prepare them?

and Step 1 4( After being quenched with ice and water (20 liters) the mixture was filtered to remove inorganic precipitates, and the organic material was extracted with ethyl acetate (15 liters))
5(The organic phase was dried over Na2SO4 and concentrated at reduced pressure to give the 3-(1-naphthoyl)indole as a crystalline solid)
These two steps are a bit difficult to understand !!
Thank you so much for replying to me, sir !!!!
 

William D.

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Yes, need clarification. In the first stage (addition of naphthoyl chloride), we make the ice-water bath or use "dry ice" to cool the flask. Step 1.3 We can add a small heat (up to 40 *C) to speed up the reaction and the best yield. At the end of time, heating can take place without reverse distillation, evaporating the excess DCM. We add water to dilute nitromethane and then the product can be extracted. We extract the product with ethyl acetate (can be replaced by other solvents) from the aqueous phase and separate the extract from an insoluble sediment (Lewis Indole complexes, which are soluble in nitromethane, but insoluble in water and ethyl acetate). Separate from the sediment, we evaporate the solvent to obtain a pure product.
 
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William D.

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In a more classic version without nitromethane and stronger Lewis acid (AlCl3), we have a large amount of side polymers (It usually looks like a rough sediment directly in the process of reaction). When using nitromethane, you can use other Lewis acid.
 

a114488

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Do you mean that other Lewis acids can be used instead of nitromethane?
 

a114488

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sir
Step1 --- 5 The organic phase was dried over Na2SO4 and concentrated at reduced pressure

Can you explain this step in detail ?
 

William D.

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sir
Step1 --- 5 The organic phase was dried over Na2SO4 and concentrated at reduced pressure

Can you explain this step in detail ?
a114488Sodium sulfate powder was added to the extract, mixed well and gave to stand. After decanted, the liquid extract from the powder and distilled. Distillation techniques under different conditions will try to publish today.
 
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a114488

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Sodium sulfate powder was added to the extract, mixed well and gave to stand. After decanted the liquid extract from the powder and distilled. Distillation techniques under different conditions will try to publish today.
William Dampier
Sir, is there any way to evaporate under reduced pressure, if there is no instrument?
 

William D.

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Oh, sure. Enough bucket with hot water and fasten a glass with a solution in it as an example.
 
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a114488

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Oh sure. Enough bucket with hot water and fasten a glass with a solution in it as an example.
William DampierOMG,It's that simple? Sir, you are so talented! Thank you very very very much

But I can't do that much at once ,,,I use 1/10 of each material for synthesis. Does the reaction time need to be reduced?
 

a114488

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and,Sir, the last question, I can’t buy nitromethane, is there anything else I can substitute?
 

William D.

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No, time does not decrease. We cannot use nitromethane, we get a product, but the yield will be lowered, and it will be more difficult to clean. Maybe you can buy 1,1,1,3,3,3-hexafluoroisopropanol (HFIP)? Although its price does not allow being the best option.
 
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aa1178251182

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No, time does not decrease. We cannot use nitromethane, we get a product, but the yield will be lowered, and it will be more difficult to clean. Maybe you can buy 1,1,1,3,3,3-hexafluoroisopropanol (HFIP)? Although its price does not allow being the best option.
William DampierSir, can HFIP replace nitromethane?
 

xiluh

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I don't understand😭
 

sirmtr

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where can i buy the raw material for this product?

what raw material costs do I have for a production of 1 kg?

can I take the raw material from europe in large quantities or do I need certain documents?
 

HIGGS BOSSON

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Where can I buy the raw material for this product?
====
All reagents are legal, they can be bought in China without documents. But I advise you to buy indole, 1-bromopentane and naphthoyl chloride in different places because in the case of a general purchase, the manager will understand for what purposes these reagents are purchased.

What raw material costs do I have for a production of 1 kg?
=====
Indole - 100 USD per kg
1-Naphthoyl chloride - 200-300USD per KG
1-bromopentane 50 USD
All other reagents for synthesis will come out at $100 per kg. Prices are approximate and depend on suppliers and purchased volumes. In Europe, prices will be twice as expensive. The cost of synthesis of 1 kg JWH-018 is about 500 dollars per kg
 
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French chocolate

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Does anyone have access to this noid ?
 

sirmtr

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is that prices in the international crisis have gone crazy, no one has access to cannabinoids in Europe in large canteens
 
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