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All 6 posts Subject: 2C-X with Red-al confirmed Please login to post Down

cilliersb
(Hive Bee)
01-07-04 08:32
No 480881
      2C-X with Red-al confirmed
(Rated as: good read)

This should come as no shock to anyone in the know, but 2,5-DiMethoxyNitrostyrene reduces in good yeild to 2C-H at ambient temp.

I used 100ml 70% red-al in Toluene with 20g nitrostyrene in 200ml (VERY DRY) toluene. Added the red-al to an additional 100ml dry toluene and added the nitrostyrene solution dropwise to the red-al while the stirrer was on high.

No inert atmosphere was used, just a drying tube and reflux condenser with a hose connected to it going out the window (not too fond of H2 build up in my kitchen). Let rund for 16 Hours after addition and did the standard red-al workup.

Ended up with 14g 2C-H, but I must admit that my working was a bit sloppy and the nitrostyrene was not of optimum purity.

No questions were ever asked about my purchase of red-al. I wouldn't buy truckloads of it though.

This is definitely the most beautiful psychedelic ever (after bromination of course)

Hope this help some beez not interrrested in using well known methods of 2C-B production.

starlight
(Hive Bee)
01-07-04 10:08
No 480886
      at what temperature

at what temperature were you able to dissolve 20g of 2,5-DMNS in 200ml of toluene?

Trying to do this at an ambient temperature of less than 15C would not work because you would not be able to get the nitrostyrene dissolved in the toluene.

cilliersb
(Hive Bee)
01-08-04 14:03
No 481166
      2C-X with Red-al confirmed

All of the Nitro did not dissolve, this was quite a pain. I have been adding it dry to a very diluted red-al in toluene sol in subsequent runs. (this worked quite well!!

starlight
(Hive Bee)
01-08-04 16:24
No 481176
      how did you get the yield you quoted above?

how did you get the yield you quoted above?

in the writeup you talk about dropwise addition - how did you achieve this with an only partially solvated substrate (without blocking the addition funnel).

Rhodium
(Chief Bee)
01-08-04 20:15
No 481213
User Picture       THF as co-solvent

Couldn't you use some THF as co-solvent to solubilize all the nitrostyrene? You can make a 10% solution of 2,5-DMNS in THF at RT.

^{The Hive - Clandestine Chemists Without Borders}

cilliersb
(Hive Bee)
01-12-04 09:08
No 481980
      Using THF

Thankx for the tip rhod.

I will try to use some THF as co-solly to see.

As for dropwise addition, this was quite a mission as the addition funnel kept getting clogged and I had to use a thin steel rod to unclog it all the time.

The point of my orig. writeup was to relay the information on the viability of Red-al as a reducing agent for the nitrostyrene, not to teach newbeez how to make 2C-B.

Just for info purposes, dehydrated CuSO4 worked well for drying the tolly and took around 24Hours.

I'll try a 30/70 THF/Toluene solvent and report back (when I have time to cook again that is.

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	All 6 posts		Subject: 2C-X with Red-al confirmed		Please login to post		Down


		cilliersb (Hive Bee) 01-07-04 08:32 No 480881				2C-X with Red-al confirmed (Rated as: good read)
						This should come as no shock to anyone in the know, but 2,5-DiMethoxyNitrostyrene reduces in good yeild to 2C-H at ambient temp. I used 100ml 70% red-al in Toluene with 20g nitrostyrene in 200ml (VERY DRY) toluene. Added the red-al to an additional 100ml dry toluene and added the nitrostyrene solution dropwise to the red-al while the stirrer was on high. No inert atmosphere was used, just a drying tube and reflux condenser with a hose connected to it going out the window (not too fond of H2 build up in my kitchen). Let rund for 16 Hours after addition and did the standard red-al workup. Ended up with 14g 2C-H, but I must admit that my working was a bit sloppy and the nitrostyrene was not of optimum purity. No questions were ever asked about my purchase of red-al. I wouldn't buy truckloads of it though. This is definitely the most beautiful psychedelic ever (after bromination of course) Hope this help some beez not interrrested in using well known methods of 2C-B production.



		starlight (Hive Bee) 01-07-04 10:08 No 480886				at what temperature
						at what temperature were you able to dissolve 20g of 2,5-DMNS in 200ml of toluene? Trying to do this at an ambient temperature of less than 15C would not work because you would not be able to get the nitrostyrene dissolved in the toluene.



		cilliersb (Hive Bee) 01-08-04 14:03 No 481166				2C-X with Red-al confirmed
						All of the Nitro did not dissolve, this was quite a pain. I have been adding it dry to a very diluted red-al in toluene sol in subsequent runs. (this worked quite well!!



		starlight (Hive Bee) 01-08-04 16:24 No 481176				how did you get the yield you quoted above?
						how did you get the yield you quoted above? in the writeup you talk about dropwise addition - how did you achieve this with an only partially solvated substrate (without blocking the addition funnel).



		Rhodium (Chief Bee) 01-08-04 20:15 No 481213				THF as co-solvent
						Couldn't you use some THF as co-solvent to solubilize all the nitrostyrene? You can make a 10% solution of 2,5-DMNS in THF at RT. ^{The Hive - Clandestine Chemists Without Borders}



		cilliersb (Hive Bee) 01-12-04 09:08 No 481980				Using THF
						Thankx for the tip rhod. I will try to use some THF as co-solly to see. As for dropwise addition, this was quite a mission as the addition funnel kept getting clogged and I had to use a thin steel rod to unclog it all the time. The point of my orig. writeup was to relay the information on the viability of Red-al as a reducing agent for the nitrostyrene, not to teach newbeez how to make 2C-B. Just for info purposes, dehydrated CuSO4 worked well for drying the tolly and took around 24Hours. I'll try a 30/70 THF/Toluene solvent and report back (when I have time to cook again that is.

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