Problem generating salt in toluene (2cb) help :(

[Babazik]

i was trying to make 2cb this days , at the last stage after bromination , i add NAOH to make 2cb go to the toluene layer (that added a bit later) , the toluene is sucked out and supposed to generate 2cbHCL when adding hcl , but instead only a black goo is generated that sinks at the bottom , i tried taking only the most concentrated toluene , from the top , and only trying to generate in it (thinking higher concentration will be easier to generate salt , and one had this problem that the drug just doenst want to generate salt in the solvent ?

 

[Babazik]

photo

 

[G.Patton]

Why do you use toluene? Try to do it by CH2Cl2 as described here.

The entire mass of acetic acid-wet salt was dissolved in warm H2O, made basic to at least pH 11 with 25 % NaOH, and extracted with 3 x 100 mL CH2Cl2. Removal of the solvent gave 33.7 g of residue, which was distilled at 115-130 °C at 0.4 mm/Hg. The white oil, 27.6 g, was dissolved in 50 mL H2O containing 7.0 g acetic acid. This clear solution was vigorous stirred, and treated with 20 mL concentrated HCl. There was an immediate formation of the anhydrous salt of 2,5-dimethoxy-4-bromophenethylamine hydrochloride (2C-B) (4). This mass of crystals was removed by filtration (it can be loosened considerably by the addition of another 60 mL H2O), washed with a little H2O, and then with several 50 mL portions of Et2O. When completely air-dry, there was obtained 31.05 g of fine white needles, with a mp of 237-239 °C with decomposition.

 

[Babazik]

Why do you use toluene? Try to do it by CH2Cl2 as described here.

G.Patton
i have a loot of goo now , i added 35% hcl to toluene and it supposed to generate 2CB hcl salt , but it doesnt form , ill check with my chemical supplier tomorrow about DCM , any idea why salt doesnt from ? , if i add hcl to toluene with 2cb it will sink as dark oil?

 

[Babazik]

Why do you use toluene? Try to do it by CH2Cl2 as described here.

G.Patton
hey i oppened a new threat with the process i hope you can help me

Novel 2cb synthesis + problems with pictures , please help me to figure it out

i've come around this novel way and tried to do it , but run into problems i hope you can help me figure it out. i've ordered 1kg of 2,5 Dmba from china. this is the steps : 1. Dissolve 8.3g (50mmol) 2,5-Dimethoxy Benzaldehyde in 50ml Methanol and 6.1g(100mmol) Nitromethane in 1L beaker. Stir...

chemforum.info

i hope you can help me there , also i have acess to DCM ' and what do you think about the reduction stage with ZINC and ipa extraction for 2ch.
thanks i hope i can figure it out.

 

[G.Patton]

what do you think about the reduction stage with ZINC

Babaziklooks simple, have you counted the yield?

 

[Babazik]

looks simple, have you counted the yield?

G.Pattonabout 45-60% from 2,5 dmba the only problem is that its needs to run at very cold conditions (about 0oC) i run it inside a freezer but ice salt bath will do , i run it at about 10oC and the 2ch comes out dark and i know it supposed to be light yellow , you can see in the IPA second pic on the left , maybe my dark 2ch came out not very good which affected the bromination and goo formation , any idea what might happen that it becomes darker at higher temp? like 10oC which isnt hot per say , ill do the reaction today at 0C like a friend told me and report back on the color.

 

[G.Patton]

any idea what might happen that it becomes darker at higher temp?

BabazikAnother way of reaction and another products. You have to check your 2C-H*HCl melting point before following reactions. The mp is 138-139 °C. Boiling point of free base is 80-100 °C at 0.4 mm/Hg.