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All 4 posts Subject: 1,4-naphthoquinone from naphthalene Please login to post Down

pHarmacist
(pHantasticant)
07-21-03 11:34
No 448798
User Picture       1,4-naphthoquinone from naphthalene
(Rated as: good read)

I'm posting this synth as the product of it serves as a staring material in the synthesis of the long-lived 2C-G-N. Also, those that are unlike me interested in MDxA synthesis can try this out and see how effective 1,4-naphthoquinone is as an oxygen donator in contrast to p-benzoquinone in Wacker process, involving donation of oxygen to the pi-bond of safrol. Advantage, as I see it, is that 1,4-naphthoquinone can bee prepared via direct oxidation of common, non-suspicious, cheap naphthalene. Make it harder for DEA.

Place a solution of 120 g (1.2 mol) of pure chromium trioxide in 150 mL of 80 per cent aqueous acetic acid in a 2-litre three-necked flask, fitted with a thermometer, mechanical stirrer and 1-litre dropping funnel. Surround the flask by a mixture of ice and salt and, when the temperature has fallen to 0 Celsius, add a solution of 64 g (0.5 mol) of pure naphtalene in 600 mL of glacial acetic acid, with constant stirring, over a period of 2-3 hours while maintaining the internal temperature at 10-15°C. Continue the stirring overnight, during which time the reaction mixture and bath attain room T. Allow the dark green solution to stand for 3 days and stirr occasionally. Pour the reaction mixture into 5-6 litres of water, collect the crude naphtoquinone by suction filtration, wash with 200 mL of water and dry in a desiccator. Recrystallise from 500 mL of petroleum ether (b.p. 80-100°C). The yield of pure 1,4-naphtoquinone, m.p. 124-125°C, is 17 g (22%) frown

Accept No Imitations, There Can Only Bee One; www.the-hive.ws

hest
(Hive Adickt)
07-21-03 11:49
No 448802
      NAphtoquinon

Juaristi, M.; Aizpurua, J. M.; Lecea, B.; Palomo, C.; CJCHAG; Can.J.Chem.; EN; 62; 1984; 2941-2944
These gues use chromiumtrioxide in acetic at 50-60°C for 120min and some 18-crown-6 ether. yeald 50%

pHarmacist
(pHantasticant)
07-21-03 11:51
No 448804
User Picture       Ok, häst

Fotgot to mention that I found the synth in Vogel's 5:th p 1022... cool

Accept No Imitations, There Can Only Bee One; www.the-hive.ws

pHarmacist
(pHantasticant)
07-28-03 15:12
No 450395
User Picture       hmm...

I could not help but to observe that my karma score increased by 0.5 after the above post (the first one), but I see no rating so that it can be found among good ones using our beloved but yet so fucking search engine...

EDIT: These gues

LOOL hest!

Do NOT disturb: Mind at Large

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	All 4 posts		Subject: 1,4-naphthoquinone from naphthalene		Please login to post		Down


		pHarmacist (pHantasticant) 07-21-03 11:34 No 448798				1,4-naphthoquinone from naphthalene (Rated as: good read)
						I'm posting this synth as the product of it serves as a staring material in the synthesis of the long-lived 2C-G-N. Also, those that are unlike me interested in MDxA synthesis can try this out and see how effective 1,4-naphthoquinone is as an oxygen donator in contrast to p-benzoquinone in Wacker process, involving donation of oxygen to the pi-bond of safrol. Advantage, as I see it, is that 1,4-naphthoquinone can bee prepared via direct oxidation of common, non-suspicious, cheap naphthalene. Make it harder for DEA. Place a solution of 120 g (1.2 mol) of pure chromium trioxide in 150 mL of 80 per cent aqueous acetic acid in a 2-litre three-necked flask, fitted with a thermometer, mechanical stirrer and 1-litre dropping funnel. Surround the flask by a mixture of ice and salt and, when the temperature has fallen to 0 Celsius, add a solution of 64 g (0.5 mol) of pure naphtalene in 600 mL of glacial acetic acid, with constant stirring, over a period of 2-3 hours while maintaining the internal temperature at 10-15°C. Continue the stirring overnight, during which time the reaction mixture and bath attain room T. Allow the dark green solution to stand for 3 days and stirr occasionally. Pour the reaction mixture into 5-6 litres of water, collect the crude naphtoquinone by suction filtration, wash with 200 mL of water and dry in a desiccator. Recrystallise from 500 mL of petroleum ether (b.p. 80-100°C). The yield of pure 1,4-naphtoquinone, m.p. 124-125°C, is 17 g (22%) Accept No Imitations, There Can Only Bee One; www.the-hive.ws



		hest (Hive Adickt) 07-21-03 11:49 No 448802				NAphtoquinon
						Juaristi, M.; Aizpurua, J. M.; Lecea, B.; Palomo, C.; CJCHAG; Can.J.Chem.; EN; 62; 1984; 2941-2944 These gues use chromiumtrioxide in acetic at 50-60°C for 120min and some 18-crown-6 ether. yeald 50%



		pHarmacist (pHantasticant) 07-21-03 11:51 No 448804				Ok, häst
						Fotgot to mention that I found the synth in Vogel's 5:th p 1022... Accept No Imitations, There Can Only Bee One; www.the-hive.ws



		pHarmacist (pHantasticant) 07-28-03 15:12 No 450395				hmm...
						I could not help but to observe that my karma score increased by 0.5 after the above post (the first one), but I see no rating so that it can be found among good ones using our beloved but yet so fucking search engine... EDIT: These gues LOOL hest! Do NOT disturb: Mind at Large

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