HIGGS BOSSON
Expert
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View attachment 6885
I am in last jwh018 steps
I got these 2 layers after heating with boiling.
Is it correct?
The top layer is JWH-018 oil
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View attachment 6885
I am in last jwh018 steps
I got these 2 layers after heating with boiling.
Is it correct?
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
Reaction scheme:
View attachment 1235
Reagents:
Indole, cas: 120-72-9
Dichloromethane, cas: 75-09-2
Tin tetrachloride, cas: 7646-78-8
1-naphthoyl chloride, cas: 879-18-5
Nitromethane, cas: 75-52-5
Ethyl acetate, cas: 141-78-6
Sodium hydroxide, cas: 1310-73-2
TBAB, cas: 1643-19-2
1-bromopentane, cas: 110-53-2
Water
Step 1. 3-(1-naphthoyl)indole.
View attachment 1236
1. To a stirring solution of indole (1000 g) in CH2Cl2(15 liters) was added SnCl4(2000 ml) in a single portion with an ice bath cooling.
2. After the ice bath was removed, the mixture was stirred at room temperature for 30 min, and then 1-naphthoyl chloride (1627 g) was added in small portions to the suspension, followed by nitromethane (10 liters).
3. The mixture was stirred for 2 h at room temperature.
4. After being quenched with ice and water (20 liters), organic material was extracted with ethyl acetate (15 liters) and the mixture was filtered to remove inorganic precipitates.
5. The organic phase was dried over Na2SO4 and concentrated at reduced pressure to give the 3-(1-naphthoyl) indole as a crystalline solid.
Step 2. 1-pentyl-3-(1-naphthoyl)indole.
View attachment 1237
1. Weigh 2000 g of the 3-(1-naphtoyl) indole, 1300 g sodium hydroxide, 800 g TBAB and add them into 10 L flask.
2. Pour 1500 g 1-bromopentane and 3000 ml of water into the flask.
3. Mix the reaction mixture, until two different layers are separated, and the entire hydroxide is dissolved.
4. When it dissolves, the flask will be heated.
5. As soon as two layers were divided and the entire hydroxide was dissolved, put the flask on the tile, and turn the heating to the maximum.
6. Install an overhead stirrer in the flask. It is necessary to mix well enough so that the layers are homogenized.
7. The overhead stirrer can work on constant stirring the entire reaction.
8. The heating at boiling continue until the contents of the flask appear to look as much as possible (several in the "milk" color), without a clear layer dedication (usually 15-30 min passes before).
9. Then remove the flask from heating and let it be to a clear separation into two layers.
10. We need the top layer. The product can crystallize directly in the flask, which makes it difficult to extract it. Therefore, we do everything quickly.
11. Remove the top layer neatly from the flasks into the glasses, or immediately into silicone forms.
12. Leave at room temperature by 24 hours until it hardens. We take silicone forms precisely for the ease of extracting the product after crystallization, it fully solidifies and takes the form, in which it was poured.
13. We take out and crush the crystallized product. Dry on paper and trays. With a warm room and ventilation, drying usually takes two days. Yield: 3000 g.
Everything at room temperature? And does the stering wheel need to be stainless steel?Reaction scheme:
View attachment 1235
Reagents:
Indole, cas: 120-72-9
Dichloromethane, cas: 75-09-2
Tin tetrachloride, cas: 7646-78-8
1-naphthoyl chloride, cas: 879-18-5
Nitromethane, cas: 75-52-5
Ethyl acetate, cas: 141-78-6
Sodium hydroxide, cas: 1310-73-2
TBAB, cas: 1643-19-2
1-bromopentane, cas: 110-53-2
Water
Step 1. 3-(1-naphthoyl)indole.
View attachment 1236
1. To a stirring solution of indole (1000 g) in CH2Cl2(15 liters) was added SnCl4(2000 ml) in a single portion with an ice bath cooling.
2. After the ice bath was removed, the mixture was stirred at room temperature for 30 min, and then 1-naphthoyl chloride (1627 g) was added in small portions to the suspension, followed by nitromethane (10 liters).
3. The mixture was stirred for 2 h at room temperature.
4. After being quenched with ice and water (20 liters), organic material was extracted with ethyl acetate (15 liters) and the mixture was filtered to remove inorganic precipitates.
5. The organic phase was dried over Na2SO4 and concentrated at reduced pressure to give the 3-(1-naphthoyl) indole as a crystalline solid.
Step 2. 1-pentyl-3-(1-naphthoyl)indole.
View attachment 1237
1. Weigh 2000 g of the 3-(1-naphtoyl) indole, 1300 g sodium hydroxide, 800 g TBAB and add them into 10 L flask.
2. Pour 1500 g 1-bromopentane and 3000 ml of water into the flask.
3. Mix the reaction mixture, until two different layers are separated, and the entire hydroxide is dissolved.
4. When it dissolves, the flask will be heated.
5. As soon as two layers were divided and the entire hydroxide was dissolved, put the flask on the tile, and turn the heating to the maximum.
6. Install an overhead stirrer in the flask. It is necessary to mix well enough so that the layers are homogenized.
7. The overhead stirrer can work on constant stirring the entire reaction.
8. The heating at boiling continue until the contents of the flask appear to look as much as possible (several in the "milk" color), without a clear layer dedication (usually 15-30 min passes before).
9. Then remove the flask from heating and let it be to a clear separation into two layers.
10. We need the top layer. The product can crystallize directly in the flask, which makes it difficult to extract it. Therefore, we do everything quickly.
11. Remove the top layer neatly from the flasks into the glasses, or immediately into silicone forms.
12. Leave at room temperature by 24 hours until it hardens. We take silicone forms precisely for the ease of extracting the product after crystallization, it fully solidifies and takes the form, in which it was poured.
13. We take out and crush the crystallized product. Dry on paper and trays. With a warm room and ventilation, drying usually takes two days. Yield: 3000 g.
@psmitty24, please have you tried to order any of the above from Alibaba? if yes do you actually get the right precusor?
Please give us some feedback after you receive and test your package. thx for the response
Received all items and made jwh18. Customers love it!
1-4 . 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.
Does this process use a separation funnel the water from the organic layer?
Hi, we ordered the 109555-87-5 direct from supplier, but they sent 83-34-1.....3-methylindole.
Could this product replace the 109555-87-5 in this synthesis?
If not is there another route using the 83-34-1 or is this product no good.
Help appriechated.
Yes, it takes to use separatory funnel in small scale synthesis
Why doesn't the result of my experiment harden after three days? The experiment was conducted in the same way, but the purity cannot be improved by recrystallizing without hardening
Actually I don't know why but some people get oily product. It has same psycho activity.
Did you proceed the same way and get the results of the solid state?
Is a batch reactor essential ? I remember previously there was no batch reactor. If they are essential now how much will a 50L batch reactor set someone back.
Any info appreciated
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