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All 7 posts Subject: distillation of 1-(2,5-dimethoxyphenyl)-2-nitroe? Please login to post Down

starlight
(Hive Bee)
12-11-03 14:22
No 476142
      distillation of 1-(2,5-dimethoxyphenyl)-2-nitroe?

is it possible to distill 1-(2,5-dimethoxyphenyl)-2-nitroethane at say 3mm hg?

Rhodium
(Chief Bee)
12-11-03 19:42
No 476212
User Picture       yup

Yes, that should be doable. Please report back the boiling point, as it is not recorded in the literature.

The Hive - Clandestine Chemists Without Borders

starlight
(Hive Bee)
12-11-03 21:38
No 476231
      1-(2,5-dimethoxyphenyl)-2-nitroethane distillation
(Rated as: good read)

the reason for distilling is that the product of the borohydride reduction was a bright red oil. This was obviously wrong and was probably due to nitrostyrene that was not clean enough. Putting this red oil into a reduction would probably make all manner of goo rather than our desired amine. Similarly I was worried that storing it would lead to degradation, so it was decided to distill straight away.

48g of this red oil was distilled at ~1mmHg (vacuum meter not sensitive enough to give a more accurate reading), and a crystal clear yellow oil distilled over at 142°C. 28g of oil were collected and what looked like 20g of black polymerised crap was left in the distillation flask (I pretty much expected this due to the very dirty nature of the starting material).

Rhodium
(Chief Bee)
12-11-03 22:00
No 476238
User Picture       Could you describe its smell?

Could you describe its smell?

The Hive - Clandestine Chemists Without Borders

starlight
(Hive Bee)
12-12-03 17:01
No 476422
      almost nothing

I was expecting to get a fruity smell similar to earlier undistilled experiments.

in fact the product was pretty close to odourless which I was surprised at.

the temperature at which the olfactory test was made was around 5 degrees C. I may be able to get more smell of it by warming it - I will see when I return to it.

What were you expecting?

Rhodium
(Chief Bee)
12-12-03 18:19
No 476431
User Picture       olfactory analysis

I have heard unconfirmed reports that the smell would be weakly hydrocarbon-like, something I find strange, as most other methoxybenzene compounds have a more or less strong fruity smell, just as you mention.

The Hive - Clandestine Chemists Without Borders

yellium
(I'm Yust a Typo)
12-12-03 22:48
No 476487
      Probably depends on purity, route of synthesis

Probably depends on purity, route of synthesis and genetic makeup of the smeller. 2,5-dimethoxythio-ethers made by the shulgin-route have a very light fruit-like smell (reminding of pears or apples), whereas if they're made using buli/alkyliodides they smell like diesel. It's a hint of something sulfourous, not really stenching but not particularly pretty.

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	All 7 posts		Subject: distillation of 1-(2,5-dimethoxyphenyl)-2-nitroe?		Please login to post		Down


		starlight (Hive Bee) 12-11-03 14:22 No 476142				distillation of 1-(2,5-dimethoxyphenyl)-2-nitroe?
						is it possible to distill 1-(2,5-dimethoxyphenyl)-2-nitroethane at say 3mm hg?



		Rhodium (Chief Bee) 12-11-03 19:42 No 476212				yup
						Yes, that should be doable. Please report back the boiling point, as it is not recorded in the literature. The Hive - Clandestine Chemists Without Borders



		starlight (Hive Bee) 12-11-03 21:38 No 476231				1-(2,5-dimethoxyphenyl)-2-nitroethane distillation (Rated as: good read)
						the reason for distilling is that the product of the borohydride reduction was a bright red oil. This was obviously wrong and was probably due to nitrostyrene that was not clean enough. Putting this red oil into a reduction would probably make all manner of goo rather than our desired amine. Similarly I was worried that storing it would lead to degradation, so it was decided to distill straight away. 48g of this red oil was distilled at ~1mmHg (vacuum meter not sensitive enough to give a more accurate reading), and a crystal clear yellow oil distilled over at 142°C. 28g of oil were collected and what looked like 20g of black polymerised crap was left in the distillation flask (I pretty much expected this due to the very dirty nature of the starting material).



		Rhodium (Chief Bee) 12-11-03 22:00 No 476238				Could you describe its smell?
						Could you describe its smell? The Hive - Clandestine Chemists Without Borders



		starlight (Hive Bee) 12-12-03 17:01 No 476422				almost nothing
						I was expecting to get a fruity smell similar to earlier undistilled experiments. in fact the product was pretty close to odourless which I was surprised at. the temperature at which the olfactory test was made was around 5 degrees C. I may be able to get more smell of it by warming it - I will see when I return to it. What were you expecting?



		Rhodium (Chief Bee) 12-12-03 18:19 No 476431				olfactory analysis
						I have heard unconfirmed reports that the smell would be weakly hydrocarbon-like, something I find strange, as most other methoxybenzene compounds have a more or less strong fruity smell, just as you mention. The Hive - Clandestine Chemists Without Borders



		yellium (I'm Yust a Typo) 12-12-03 22:48 No 476487				Probably depends on purity, route of synthesis
						Probably depends on purity, route of synthesis and genetic makeup of the smeller. 2,5-dimethoxythio-ethers made by the shulgin-route have a very light fruit-like smell (reminding of pears or apples), whereas if they're made using buli/alkyliodides they smell like diesel. It's a hint of something sulfourous, not really stenching but not particularly pretty.

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