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All 4 posts Subject: THF -> GBL query Please login to post Down

kidamnesiac
(Stranger)
05-19-04 03:37
No 508129
      THF -> GBL query

SWIM was thinking of doing a THF>GBL synth as per https://www.rhodium.ws/pdf/solventfree.kmno4.oxidation.pdf
and was wondering if any other bees had an experience with this as upon taking a gander @ 2mmol of THF in relation to ~4 grams of KMnO4 and CuSO4*5H2O it became apparent that the THF would be but a drop into a pile of macerated oxiderizer. Could anybee comment on whether this scale is wrong as SWIM was thinking of doing it 4mol THF to 1mol KMnO4 along the molar ratio lines and had a dream about the experiment that ended in him awaiting for an opportunity to distill and analyze the product. thank ye in advance.

ning
(acetaminophanatic)
05-20-04 05:47
No 508368
User Picture       There are other methods of doing this.

There are other methods of doing this.

The CuSO4.5H2O supplies water for the oxidation, and may also somehow mediate the oxidation.

I recommend trying some kind of halogen-based oxidation. TCCA is the ever-popular agent for this. There's threads on the topic. Basically, doing an acidic oxidation should work, as halogen is the real oxidizing agent. Much room for research in this area.

Failing that, I could look something up for you. I have a couple papers involving this sort of oxidation.

_{...it's an AOL chatroom for dyslexic spider monkies...}

Aurelius
(Active Asperger Archivist)
05-20-04 11:04
No 508410
      Methods

If you want a variety of methods to GBL/GHB, try this:

Post 439780 (Aurelius: "Compilation on GHB/GBL", Methods Discourse)

Act quickly or not at all.

kidamnesiac
(Stranger)
05-21-04 23:50
No 508678
      GC-MS data

SWIM's GC-MS analysis of the crude product revealed butyrolactone as 7% of final product after extraction with ethyl acetate. distillation to follow.
it looks like a lot of the THF was simply broken up into butanol and a furan-one of undeterminable structure, which is definitely not an over-oxidized product.
stay tuned...

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	All 4 posts		Subject: THF -> GBL query		Please login to post		Down


		kidamnesiac (Stranger) 05-19-04 03:37 No 508129				THF -> GBL query
						SWIM was thinking of doing a THF>GBL synth as per https://www.rhodium.ws/pdf/solventfree.kmno4.oxidation.pdf and was wondering if any other bees had an experience with this as upon taking a gander @ 2mmol of THF in relation to ~4 grams of KMnO4 and CuSO4*5H2O it became apparent that the THF would be but a drop into a pile of macerated oxiderizer. Could anybee comment on whether this scale is wrong as SWIM was thinking of doing it 4mol THF to 1mol KMnO4 along the molar ratio lines and had a dream about the experiment that ended in him awaiting for an opportunity to distill and analyze the product. thank ye in advance.



		ning (acetaminophanatic) 05-20-04 05:47 No 508368				There are other methods of doing this.
						There are other methods of doing this. The CuSO4.5H2O supplies water for the oxidation, and may also somehow mediate the oxidation. I recommend trying some kind of halogen-based oxidation. TCCA is the ever-popular agent for this. There's threads on the topic. Basically, doing an acidic oxidation should work, as halogen is the real oxidizing agent. Much room for research in this area. Failing that, I could look something up for you. I have a couple papers involving this sort of oxidation. _{...it's an AOL chatroom for dyslexic spider monkies...}



		Aurelius (Active Asperger Archivist) 05-20-04 11:04 No 508410				Methods
						If you want a variety of methods to GBL/GHB, try this: Post 439780 (Aurelius: "Compilation on GHB/GBL", Methods Discourse) Act quickly or not at all.



		kidamnesiac (Stranger) 05-21-04 23:50 No 508678				GC-MS data
						SWIM's GC-MS analysis of the crude product revealed butyrolactone as 7% of final product after extraction with ethyl acetate. distillation to follow. it looks like a lot of the THF was simply broken up into butanol and a furan-one of undeterminable structure, which is definitely not an over-oxidized product. stay tuned...

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