AB-001 is pretty potent indole based cannabinoid with adamantane linker
Here is our formula what we need!
Ingridients:
1-Adamantanecarbonyl chloride (250 grams for yield of AB-001 reagent 25g maybe lose to 15g )
Tin chloride IV(for gram of adamantane we add about 0,5l or 500ml, we should have 1250 liters of SnCL4)
Ethyl acetate(we need 500ml)
Indole(625g)
MgSO4(as drying agent, you can use sodium sulfate)
DCM(about 1625L)
Nitromethane(812,5ml)
Water(1625L)
ATTENTION: I RECOMMENDING DOING YOU PROPORTIONS BECAUSE FOR ME IT WORKED, BUT FOR SOMEONE CAN COMPLAIN THAT THERE IS SMALL AMMOUNT AND IT WILL NOT HAVE 20g, FOR ME IT WORKED, FOR YOU DON'T KNOW, SO I RECOMMEND YOU CHANGE A PROPORTION, SO IN SYNTHESIS I DON'T ADD MY PROPORTIONS, THE ABOVE IS MY PROPORTIONS WHICH IS I RECOMMEND TO CHANGE!
Synthesis time:
1.SnCL4 is added in flask with indole solution in DCM.
2.Give a stir for 25 minutes-30 minutes, after you got room temperature, then the adamantanecarbonyl chloride is added in small portions along with nitromethane.
3.The melting point of adamantanecarbonylchloride is 49-51, heating up on temperature 50*C for 2 hours do not forget teflone magnet, it should heating up and mix.
4.After 2 hours passed, the reaction mixture we load our very cold water, now we filtrate to remove inorganic trash from mixture, layers should be separated.
5.The water layer we extracting with ethyl acetate, and extract is combined with extract.
6.The final one, we drying organic substance in MgSO4 or sodium sulfate is can work too, should be concentrated at pressure, ATTENTION: reduced
We collecting crystaline adamantane indole
Time for preparing a AB-001:
We adding in flask a NaOH.
We add water in flask.
Now the adamantane indole we pouring in flask.
After loading 1-bromopentane aka amyl bromide.
Mix thoroughly.
Placing on hotplate adding the teflone magnet, the temperature is 50*C.
Now we need wait when adamantane indole is melted into liquid phase.
Two layers appears, after 5 minutes place on table from a hotplate.
Waiting when the flask and mixture is a room temperature, cleaning with water, DO NOT ADD COLD WATER unlike TMCP or Naphtoyl indoles the adamantane indole will be crystilisied in seconds!
Pouring in beaker, and we are adding the AB-001 layer into other beaker using needle to collect.
Once it's crystailzied it's about 5 hours.
We are doing recrystalization of the AB-001.
We pouring IPA/Ethyl acetate/maybe acetone will work but ain't tested i think no.
So now we hitting on temperature about 55*C, after the crystaline thing is dissolved in solvents that i nammed.
Wait until it will be crystalized.
After with the glass stick we breaking big crystals, now we filtrate using a vacuum filtration, i recommend to wash with IPA.
Done.
Here is our formula what we need!
Ingridients:
1-Adamantanecarbonyl chloride (250 grams for yield of AB-001 reagent 25g maybe lose to 15g )
Tin chloride IV(for gram of adamantane we add about 0,5l or 500ml, we should have 1250 liters of SnCL4)
Ethyl acetate(we need 500ml)
Indole(625g)
MgSO4(as drying agent, you can use sodium sulfate)
DCM(about 1625L)
Nitromethane(812,5ml)
Water(1625L)
ATTENTION: I RECOMMENDING DOING YOU PROPORTIONS BECAUSE FOR ME IT WORKED, BUT FOR SOMEONE CAN COMPLAIN THAT THERE IS SMALL AMMOUNT AND IT WILL NOT HAVE 20g, FOR ME IT WORKED, FOR YOU DON'T KNOW, SO I RECOMMEND YOU CHANGE A PROPORTION, SO IN SYNTHESIS I DON'T ADD MY PROPORTIONS, THE ABOVE IS MY PROPORTIONS WHICH IS I RECOMMEND TO CHANGE!
Synthesis time:
1.SnCL4 is added in flask with indole solution in DCM.
2.Give a stir for 25 minutes-30 minutes, after you got room temperature, then the adamantanecarbonyl chloride is added in small portions along with nitromethane.
3.The melting point of adamantanecarbonylchloride is 49-51, heating up on temperature 50*C for 2 hours do not forget teflone magnet, it should heating up and mix.
4.After 2 hours passed, the reaction mixture we load our very cold water, now we filtrate to remove inorganic trash from mixture, layers should be separated.
5.The water layer we extracting with ethyl acetate, and extract is combined with extract.
6.The final one, we drying organic substance in MgSO4 or sodium sulfate is can work too, should be concentrated at pressure, ATTENTION: reduced
We collecting crystaline adamantane indole
Time for preparing a AB-001:
We adding in flask a NaOH.
We add water in flask.
Now the adamantane indole we pouring in flask.
After loading 1-bromopentane aka amyl bromide.
Mix thoroughly.
Placing on hotplate adding the teflone magnet, the temperature is 50*C.
Now we need wait when adamantane indole is melted into liquid phase.
Two layers appears, after 5 minutes place on table from a hotplate.
Waiting when the flask and mixture is a room temperature, cleaning with water, DO NOT ADD COLD WATER unlike TMCP or Naphtoyl indoles the adamantane indole will be crystilisied in seconds!
Pouring in beaker, and we are adding the AB-001 layer into other beaker using needle to collect.
Once it's crystailzied it's about 5 hours.
We are doing recrystalization of the AB-001.
We pouring IPA/Ethyl acetate/maybe acetone will work but ain't tested i think no.
So now we hitting on temperature about 55*C, after the crystaline thing is dissolved in solvents that i nammed.
Wait until it will be crystalized.
After with the glass stick we breaking big crystals, now we filtrate using a vacuum filtration, i recommend to wash with IPA.
Done.