Sinteza AM-694 z Grignardovo reakcijo

[William D.]

Korak 1:

1. Suspenziji 1,00 g 2-jodobenzojske kisline v 30 ml diklorometana pri 0 *C smo po kapljicah dodali 4,00 g oksaliliklorida.
2. Reakcijsko zmes smo segreli na sobno temperaturo in jo mešali 2 uri.
3. Po ohladitvi smo v vakuumu odstranili topilo in odvečni oksaliliklorid ter dobili rjav ostanek (0,90 g), ki smo ga brez nadaljnjega čiščenja uporabili v naslednjem koraku.
4. 1,40 g indola v 5,0 ml etra smo pri 0 *C kapljično dodali mešani raztopini 3,17 ml 2,5M etilmagnezijevega bromida v etru, razredčeni z 1,1 ml etra.
5. Raztopino smo 0,5 h mešali pri sobni temperaturi, nato pa smo po kapljicah dodali raztopino 0,90 g 2-jodobenzojklorida v 5 ml etra.
6. Reakcijsko zmes smo mešali 1,5 h, gasili z nasičenim vodnim amonijevim kloridom in mešali, dokler trdna snov ni razpadla v fino suspenzijo.
7. Ostanek smo sprali z vodo in etrom, nato pa ga suspendirali v 20 ml metanola, ki smo mu dodali 4 g natrijevega hidroksida in 10 ml vode.
8. Mešanico smo pri sobni temperaturi mešali 18 ur, nato smo trdno snov filtrirali in sperli z zaporednimi odmerki metanola, vode in etra.
9. Sušenje v vakuumu pri 100 *C je 1,06 g (70 %) 3-(2-jodobenzoil)indola spremenilo v viskozno olje, ki je bilo uporabljeno v naslednjem koraku brez nadaljnjega čiščenja.


Korak 2:

1. Raztopini 1,06 g 3-(2-jodobenzojl)indola v 10,0 ml N, N-dimetilformamida dodamo 0,5 g natrijevega hidrata.
2. Reakcijsko zmes smo mešali pri sobni temperaturi in počasi dodali 1,03 g 1-bromo-5-fluoropentana.
3. Raztopino smo pri 120 *C mešali 1 uro.
4. Po ohladitvi smo reakcijsko zmes razredčili z vodo in ekstrahirali s tremi odmerki etilacetata.
5. Ekstrakte smo izprali s slanico in posušili, topilo pa smo odstranili v vakuumu.
6. Izdelek 0,60 g (30 %) 1-(heptil-7-karboksilata)-3-(2-jodobenzojl)indola kot rumene trdne snovi.

 

[Barter]

The synthesis says it makes 1-(heptyl-7-carboxylate)-3-(2-iodobenzoyl)indole, but it should be 1-(5-fluoropentyl)-3-(2-iodobenzoyl)indole (AM-694) based on 1-bromo-5-fluoropentane. No way that reagent adds a heptyl or carboxylate group. Looks like a mix-up—can you clarify the synthesis path?
Thanks

 

[loadingST]

I also have seen such misslabelings in chemicals that comed as synthetic canabinoids, on the image path all is clear but the think im seeing is the canabinoids that come from china was euphoric and strong, and now all this canabinoids made by this way or by kits are actualy less euphoric then thc, im almost shure here is a big lie that we normal people dont know, but from where comes the difference ?

 

[HIGGS BOSSON]

If synthetic cannabinoid is weaker than THC, then it was synthesized with errors. The JWH series is much stronger than THC, maybe it's not always more euphoric, but many people like the powerful action of synthetics. Still, THC is milder.

 

[loadingST]

I remember when taking the first china adb-butinaca, 5f-sgt-151,am-2201, and some other i have tried from china and they were actualy so euphoric like third eye happines/euphoria 8/10 euphoria 8/10 sedation(thry were china stock but shiped from spain buyjwh if you remember them, and i tried the greece flyrc products first and was so disapointed, and recently tried a 5f i think, and that was not only not strong, but and making me feel so bad, normal thc is 5/10 euphoria and 3/10 sedation lets say for me when i dont have tolerance and all the newer ones made by the chinese precursors are so weak and i cant figure out why just zero euphoria, thats not how canabinoids are supposed to fell from my experience, i still havent tried to made a canabinoid but im a big enthusiast of FC or grignard so i must try haha

 

[Barter]

@HIGGS BOSSON The synthesis claims to produce 1-(heptyl-7-carboxylate)-3-(2-iodobenzoyl)indole, but it should actually result in 1-(5-fluoropentyl)-3-(2-iodobenzoyl)indole (AM-694) using 1-bromo-5-fluoropentane. It's unlikely that this reagent would introduce a heptyl or carboxylate group. It seems like there might be a mix-up—could you clarify the synthesis route? Thank you!