JWH-018 synthesis. Small scale.

[WillD]

Reaction scheme:

​

Reagents:

• Indole (cas 120-72-9) 0.117 g;
• Aluminum oxide (Al2O3) 1 g;
• 1-Naphthoyl chloride (cas 879-18-5) 0.286 g;
• Sodium carbonate (Na2CO3) 0.16 g;
• 1-Bromopentane (cas 110-53-2) 0.18 g;
• Ethanol (EtOH) 60 ml;
• Distilled water;

Equipment and glassware:

• Microwave vial 5 ml;
• Microwave oven;
• Beakers 10 mL x2;
• Glass rod and spatula;
• Heating plate;
• Freezer;
• Vacuum source (optional);
• Schott filter and Buchner flask (optional);

Synthesis:

1. Indole 0.117 g is mixed with aluminum oxide (Al2O3) 1 g and mixed together until a homogeneous powder is formed.
2. 1-Naphthoyl chloride 0.286 g is added to the mixture and stirred to evenly mixed solution.
3. The final mixture is irradiated at 100 °С (400 W) for 8 minutes in a sealed 5 ml microwave vial.
4. The vial is cooled to a room temperature. Sodium carbonate (Na2CO3) 0.16 g as a finely ground powder and 1-bromo-pentane 0.18 g are added into the vial and then stirred to evenly mixed solution.
5. The resulting mixture is irradiated again in the microwave reactor (vial) at 100 °C (400W) for 4 minutes.
6. Then, ethanol (EtOH) 60 ml is added to the reaction mixture and refluxed for 20 minutes.
7. Aluminum oxide (Al2O3) is filtered and washed with distilled water 15 ml twice, and dried for next batch.
8. Ethanol solution (EtOH) with JWH-018 is treated with water 10 ml, placed in a freezer and crystalline JWH-018 is formed. Product is filtered on a Schott funnel and Buchner flask.

JWH-018 can be used as liquid.​

 

[jexana23]

I m a novice , can you explainbetter, i search for indole and i found many tipes of indole and my brain go down
How much quantyti etc.

 

[jexana23]

Can you explain for stupit noob people like me , i know i m very stupid but if you explain for noobs i think it a possible to understand

 

[HEISENBERG]

CAS 120-72-9

 

[nutritiousforeach]

Why is irradiation specifically used, instead of normal controlled heating at 100*C? Just wanted to understand the chemistry. Thank you.

 

[WillD]

Microwave radiation catalyzes many reactions and sometimes change the direction. Relatively new and promising sphere

 

[krtl91]

hi there . thank you for information. what can i use instead of 1 naphtoyl chloride ? i cant find it commercially here . or how can i make for my self ? thx

 

[WillD]

1-naphthoyl chloride substituted - 4-methoxy or 4-ethyl -1-naphthoyl chlorides. 1-Adamantanecarbonyl chloride, 2-Iodobenzoyl chloride, 2,2,3,3-Tetramethylcyclopropanecarbonyl chloride, etc

 

[Khaled]

The substitute for naphthoyl chloride is benzoyl chloride 99%.

 

[krtl91]

thank you so much

 

[krtl91]

is there one which i could find commercially available easier than others ? thank you

 

[krtl91]

hi there .Thank you for your time . İ am having trouble to find those reagents commercially available. Which one of those i can synthesis myself from the commercially available ones (as a amateur one i would prefer to easiest one ) thank you .

 

[WillD]

You can find acid, not chloride (for example naphthoyl acid) and make chloride with thionyl chloride or phosphoryl chloride. Synthesis (click). You can use other acids, by analogy.

 

[krtl91]

none of them İ mean literally none of them available commercially in my frkng country. ı guess ı ll just order napthoyl cloride from chına or somewhere and do the procedure . coz ı assume as a amateur ıt doesnt worth to that much trouble to optaın naphtoyl chlorıde when ıts avaılable commercially ın other countrıes

 

[WillD]

Yes, of course it is better to buy chloride than to make it, not the most pleasant procedure.

 

[Khaled]

The substitute for naphthoyl chloride is benzoyl chloride 99%.

 

[northenos]

What equipment needed to microwave synthesis ?

 

[WillD]

MW oven, beakers, scales, grinders, filters, etc.
PS: Who synthesizes ADBB-noids with main reagent (with potassium carbonate), can try this synthesis starting from step 4

 

[阿卡Mario]

1. can sealed bottles explode? 2. is a microwave oven good for home use?

 

[northenos]

I still confused start step 6, what equipment needed to reflux ?
any video to explain that ?

 

[northenos]

After reflux, the mixture filtered and the filter washed with water twice ? How to wash that i need example, and step 8 i still confused with the word “EtOH phase”, what is EtOH phase ?

 

[ASheSChem]

i think you need to read and read the forum

http://bbzzzsvqcrqtki6umym6itiixfhni37ybtt7mkbjyxn2pgllzxf2qgyd.onion/index.php?threads/reflux-and-heating-techniques.589/

 

[northenos]

Thank you