JWH-018 synthesis

[WillD]

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.

 

[aa1178251182]

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?

 

[Claudio51]

Sir, can HFIP replace nitromethane?

aa1178251182I noticed that you do not use the column to purify the products ... which purification method do you use ?

 

[Claudio51]

I noticed that you do not use the column to purify the products ... which purification method do you use ?

Claudio51I noticed that you do not use the column to purify the products ... which purification method do you use ?

 

[charmingcho]

What if the finally made jwh-018 doesn't harden?
And if it's hardened, what solvent should I use to recrystallize it to increase the purity?
Recrystallization was not done well with the IPA.

 

[HerrHaber]

Looks like partial polymerization that occured by accident, contaminated your product to the point where crystalization is impeded. The suggestion I may have just by pure reasoning is dissolving the product in a solvent that is absolutely unwelcoming solvation medum for the suspected polymer (no clue whatever polycycles may form into a complex matrix but polymers often are insoluble in certain media) I would start with the most stricti selective solvent for the product alone and that if there is something left behind is not of interest. I'm sure people with applied experience with this particular compound should know a variety of purification tricks but if the quantity is in such manner I would do a DCVC on it even if I would optimize the elution scheme by theory using what others observed before performing the separation.

P.S. thre's a youtube video on dcvc which is a suitable method of prep chromatography if you want pure stuff (just search for it)

 

[beginner]

what is the concentration of Tin (IV) chloride please ?

 

[Claudio51]

Reaction scheme:​

View attachment 1235 ​

Equipment and glassware:

• 50 L Batch reactor, which is equipped with drip funnel, top stirrer, thermometer, temperature control system (cooling) and reflux condenser;
• 10 L Flask;​
• Retort stand and clamp for securing apparatus (optional);​
• Reflux condenser;​
• Top stirrer;​
• Heating plate;​
• Funnel;​
• Several buckets 25 L;​
• Beaker 2000 mL;
• Pyrex dishes;
• Vacuum source;
• Scale;
• Measuring cylinder 1000 mL;
• Glass rod and spatula;
• Scoops;
• Nutsche filter;
• Rotary evaporator;

Reagents: View attachment 7133 ​

• 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.​

View attachment 1236 ​

I noticed that you do not use the column to purify the products ... which purification method do you use ?​

William Dampier

 

[charmingcho]

It says it's separated into two layers, but I'm separated into three layers. The oil layer, the water layer, and the solid sink. Is this solid the material I want? And I'm trying to harden the oil layer, but it doesn't harden no matter how much time passes.

 

[readytorock]

Hello .
One question I have, I may have heard wrong. Does it release hydrogen gases during synthesis?