Syntéza AM-694 prostredníctvom Grignardovej reakcie

[William D.]

Krok 1:

1. K suspenzii 1,00 g kyseliny 2-jódobenzoovej v 30 ml dichlórmetánu pri 0 *C sa po kvapkách pridali 4,00 g oxalylchloridu.
2. Reakčná zmes sa zahriala na izbovú teplotu a miešala sa 2 h.
3. Po ochladení sa rozpúšťadlo a prebytočný oxalylchlorid odstránili in vacuo, čím sa získal hnedý zvyšok (0,90 g), ktorý sa použil v ďalšom kroku bez ďalšieho čistenia.
4. K miešanému roztoku 3,17 ml 2,5M etylbromidu horečnatého v éteri, zriedenému 1,1 ml éteru, sa pri 0 *C po kvapkách pridalo 1,40 g indolu v 5,0 ml éteru.
5. Roztok sa miešal 0,5 h pri izbovej teplote a po kvapkách sa pridal roztok 0,90 g 2-jódbenzoylchloridu v 5 ml éteru.
6. Reakčná zmes sa miešala 1,5 h, uhasila sa nasýteným vodným roztokom chloridu amónneho a miešala sa, kým sa pevná látka nerozpadla na jemnú suspenziu.
7. Zvyšok sa premyl vodou a éterom, potom sa suspendoval v 20 ml metanolu, ku ktorému sa pridali 4 g hydroxidu sodného a 10 ml vody.
8. Zmes sa miešala pri izbovej teplote 18 h, tuhá látka sa odfiltrovala a premyla postupnými dávkami metanolu, vody a éteru.
9. Sušením vo vákuu pri 100 *C sa z 1,06 g (70 %) 3-(2-jodobenzoyl)indolu stal viskózny olej, ktorý sa použil v ďalšom kroku bez ďalšieho čistenia.


Krok 2:

1. K roztoku 1,06 g 3-(2-jodobenzoyl)indolu v 10,0 ml N, N-dimetylformamidu sa pridalo 0,5 g hydrátu sodného.
2. Reakčná zmes sa miešala pri izbovej teplote a pomaly sa pridalo 1,03 g 1-bróm-5-fluórpentánu.
3. Roztok sa miešal pri 120 *C počas 1 h.
4. Po ochladení sa reakčná zmes zriedila vodou a extrahovala tromi dávkami etylacetátu.
5. Extrakty sa premyli soľným roztokom, vysušili a rozpúšťadlo sa odstránilo vo vákuu.
6. Výťažok 0,60 g (30 %) 1-(heptyl-7-karboxylátu)-3-(2-jódbenzoyl)indolu ako žltá tuhá látka.

 

[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!