quinone from Hydroquinone using hydrogen peroxide

[budstealth]

55 g of hydroquinone, 115 g of isopropyl alcohol as a reaction medium, and 1 g of iodine as a catalyst were charged into a 300 ml four-necked glass reaction vessel with a stirrer, a dropping funnel, and a thermometer. Then stirring was started, and after 58 g of a 35% hydrogen peroxide solution were added over about 3 hours while keeping the temperature at 30-35°C, the temperature was raised to about 45°C, which was kept for about 3 hours to complete the reaction. After the completion of the reaction, the reaction mixture was cooled gradually to about 15°C, and the reaction product was filtered by suction. The reaction product was washed with a small amount of isopropyl alcohol, and dried under reduced pressure to yield 49.5 g of p-benzoquinone. The yield was 91.6% (based on the charged hydroquinone, hereinafter the same being applied), the melting point was 111-112°C, and the purity as measured by HPLC was 99.0%.

The filtered mother liquor containing isopropyl alcohol that had been obtained by filtering the reaction product by suction was distilled under normal pressures or reduced pressure in a usual manner to recover aqueous isopropyl alcohol containing about 12% of water. The recovered isopropyl alcohol can be used again as a reaction medium in the next reaction.

Is iodine really needed?  And if iodine is needed is there a source of iodine that can be bought in a grocery store or similar?  I read Bond_DoubleBond Benzo Bees reaction and think that no iodine is needed if heat is used as the catalyst.  Just IMO... What do you think?

[terbium]

For OTC iodine look search in the Stimulants Forum, there are procedures described there for obtaining iodine from tincture of iodine, or perhaps you could use the tincture of iodine directly in place of the iodine.

[budstealth]

Saw that post and very interesting... is there a reason people make it OTC instead of just ordering it from a chemical supply?  Its not watched, is it?  But i still need to know if iodine is even needed.

[Rhodium]

Iodine is a List II chemical.

[homeslice]

Post 473279

(Bond_DoubleBond: "Big Breakthrough for Benzo Bees", Methods Discourse)

Swim had all sorts of problems with that synth that you mentioned. Try this one instead, also it calls for much less iodine. Just extract some tincture using h2o2, or check the local pet shops for a pint of 7% i2. Swim tried about 5 shops til he found a store that had 6 pints. Swim took em all one by one with a friend  

[Mercury]

Iodine is a List II chemical.

So is Acetone, but it's sold in hardware stores across the US   .

Iodine can easily be extracted from veterinary Iodine 7% tincture.

[budstealth]

Still avoiding the question.  Is Iodine needed? I mean if i have a day or two to spare(dont think it would take that long anyways) whats wrong with just not using iodine as a catalyst... I also see that the iodine ends up in the benzo crystals as posted above, his decant was all ipa and no iodine so where did it end up, i suppose in the benzo crystals.

[moo]

Still avoiding the question.  Is Iodine needed?

I'm convinced that it is, but if you test the reaction without iodine and end up with benzoquinone then it's all good.

[Ziqquratu]

This is my own theory, and may be entirly wrong... I think that, perhaps, the iodine may in fact act as the direct oxidant, oxidizing hydroquinone to benzoquinone and being reduced to I^- in the process.  The hydrogen peroxide then reoxidizes the I^- to I₂ and so the cycle continues...

Please, someone correct me if I've got it wrong.

[moo]

Exactly.

[homeslice]

his decant was all ipa and no iodine so where did it end up, i suppose in the benzo crystals

The I2 dissolves in the ISA, and thats why the decant is such a dark red. Swim doesnt seem to see any orange or red in the benzo crystals. They are bright yellow. They had some traces of the red isa on em but after washing with regular isa, they quickly turn bright yellow.

Is it really so hard to come up with 1g of i2 for 150g of benzo?

[moo]

Especially when it can be made from KI or NaI with hydrogen peroxide, UTFSE.