NOCAINE/CPCA:
A refined synthesis.
By mewnmewamine!! (Dats me!!! :333 ^^^w^^^)
I realise there is already a synthesis on this forum (just copied from rhodium ig) however it has many issues the improvements are as follows:
•SWIM has actually tried it and had success
•I have a preparation prepared for all the reagents *that you cant find online*
•Ive added a reagent list
•Ive actually named the fucking compound im making
rather than just calling it a cocaine analog
•ive added sidenotes from SWIMs personal experience
Any questions ill be happy to answer :3
REAGENT LIST
111g bromoaniline (or another way to get brclbenzene)
270ml water
510ml 37% hcl
48g sodium nitrite
93.16g cupric chloride
1l acetone
53.5g magnesium
2.8l THF
Some NaOH for basifying
Some extra HCl for acidifying
Around 30g arecoline HBr
Some solvents for extraction
P-BROMOCHLOROBENZENE
Combine 111g of bromoaniline and 171 mL of distilled water in a 1l beaker. Place the beaker on a magnetic stirrer, and slowly add 171 mL of 37% hydrochloric acid .
Once the fumes subside, place the beaker in a salt-ice bath
Once the mixture reaches 0°C, begin to add a solution of 48g of sodium nitrite in 99 mL of h2o dropwise.
^°^=^=^^^
Mew sidenote: "Keep it all at 5 °C or less °w° until you are told otherwise"
^°^=^=^^^
Meanwhile, dissolve 83.16g of cupric chloride in 339 mL of 37% hydrochloric acid in a 2L RBF. Place the flask in a salt-ice bath and wait until it reaches 0°C
When the sodium nitrite addition is complete let it stir for a few mins. . Then slowly add that sol to the cupric chloride sol.
Remove the ice bath and allow the mixture to come to RT.
Once the mixture reaches room temperature the solution is slowly heated to 60°c and kept there until no nitrogen oxides fumes are evolved
The solvent is removed in vacuo and 1l acetone is added, the solution is filtered and the solvent removed in vacuo to yield p-bromochlorobenzene
CHLOROPHENYLMAGNESIUMBROMIDE
53.5 g of magnesium turnings (2.2 mol) and a bit of iodine are charged into a 3l two necked rbf at RT under argon.
^°^=^=^^^
mew sidenote here :3 : "the argon aint too important just keep everything super fucking dry it can also be replaced by nitrogen or the even easier to get helium you jusy gotta have helium constantly running cos its light n blows away.
Easily worst noble gas but it is easy to get so
¯\_(ツ)_/¯
"
^°^=^=^^^
The mixture is then heated to 70°C and a solution of 404g 1-bromo-4-chlorobenzene in 2l THF is added dropwise over 1hr after addition the mixture is heated to reflux for 30mins its cooled to 20°c poured into a glass bottle and sealed for later this solution is around 1M i
^°^=^=^^^
Another mew sidenote here :3 " you can use ether too as both ether and thf are widely available i just used thf as its what was on hand
^°^=^=^^^
NOCAINE
The arecoline was basified using 25% ammonia .
To a solution of 250ml of 1M 4-chlorophenylmagnesium bromide in 500ml THF was added 19.35g of arecoline freebase in 300ml THF (at -10°C to -20°C) over 30mins or so
(This is easily reached with CaCl+ice).
Stir for 30 mins keeping the solution at same temp,Next an eyeballed amount of ice was added and the solution was acidified with hcl.
The aqueous layer was separated, washed with ether, sat NaCl sol and the solution is basified.
Then solution was extracted with ether, washed with sat NaCl sol, dried, and concentrated in vacuo.
This was recrystallised from boiling ethyl acetate :3
I do not currently have pics but if SWIM had the funds to reattempt they would make a video of the process.
A refined synthesis.
By mewnmewamine!! (Dats me!!! :333 ^^^w^^^)
I realise there is already a synthesis on this forum (just copied from rhodium ig) however it has many issues the improvements are as follows:
•SWIM has actually tried it and had success
•I have a preparation prepared for all the reagents *that you cant find online*
•Ive added a reagent list
•Ive actually named the fucking compound im making
rather than just calling it a cocaine analog•ive added sidenotes from SWIMs personal experience
Any questions ill be happy to answer :3
REAGENT LIST
111g bromoaniline (or another way to get brclbenzene)
270ml water
510ml 37% hcl
48g sodium nitrite
93.16g cupric chloride
1l acetone
53.5g magnesium
2.8l THF
Some NaOH for basifying
Some extra HCl for acidifying
Around 30g arecoline HBr
Some solvents for extraction
P-BROMOCHLOROBENZENE
Combine 111g of bromoaniline and 171 mL of distilled water in a 1l beaker. Place the beaker on a magnetic stirrer, and slowly add 171 mL of 37% hydrochloric acid .
Once the fumes subside, place the beaker in a salt-ice bath
Once the mixture reaches 0°C, begin to add a solution of 48g of sodium nitrite in 99 mL of h2o dropwise.
^°^=^=^^^
Mew sidenote: "Keep it all at 5 °C or less °w° until you are told otherwise"
^°^=^=^^^
Meanwhile, dissolve 83.16g of cupric chloride in 339 mL of 37% hydrochloric acid in a 2L RBF. Place the flask in a salt-ice bath and wait until it reaches 0°C
When the sodium nitrite addition is complete let it stir for a few mins. . Then slowly add that sol to the cupric chloride sol.
Remove the ice bath and allow the mixture to come to RT.
Once the mixture reaches room temperature the solution is slowly heated to 60°c and kept there until no nitrogen oxides fumes are evolved
The solvent is removed in vacuo and 1l acetone is added, the solution is filtered and the solvent removed in vacuo to yield p-bromochlorobenzene
CHLOROPHENYLMAGNESIUMBROMIDE
53.5 g of magnesium turnings (2.2 mol) and a bit of iodine are charged into a 3l two necked rbf at RT under argon.
^°^=^=^^^
mew sidenote here :3 : "the argon aint too important just keep everything super fucking dry it can also be replaced by nitrogen or the even easier to get helium you jusy gotta have helium constantly running cos its light n blows away.
Easily worst noble gas but it is easy to get so
¯\_(ツ)_/¯"^°^=^=^^^
The mixture is then heated to 70°C and a solution of 404g 1-bromo-4-chlorobenzene in 2l THF is added dropwise over 1hr after addition the mixture is heated to reflux for 30mins its cooled to 20°c poured into a glass bottle and sealed for later this solution is around 1M i
^°^=^=^^^
Another mew sidenote here :3 " you can use ether too as both ether and thf are widely available i just used thf as its what was on hand
^°^=^=^^^
NOCAINE
The arecoline was basified using 25% ammonia .
To a solution of 250ml of 1M 4-chlorophenylmagnesium bromide in 500ml THF was added 19.35g of arecoline freebase in 300ml THF (at -10°C to -20°C) over 30mins or so
(This is easily reached with CaCl+ice).
Stir for 30 mins keeping the solution at same temp,Next an eyeballed amount of ice was added and the solution was acidified with hcl.
The aqueous layer was separated, washed with ether, sat NaCl sol and the solution is basified.
Then solution was extracted with ether, washed with sat NaCl sol, dried, and concentrated in vacuo.
This was recrystallised from boiling ethyl acetate :3
I do not currently have pics but if SWIM had the funds to reattempt they would make a video of the process.