GHB-->GBL

[foxy2]

Will a strong acid convert GHB--->GBL???
SWIM is deviseing a clean-up procedure for gheto GHB.
If this reactor goes a short series of solvent/water extractions while converting the corresponding compounds should effectively clean up ghetto GHB.

Is there any other simple way to go from GHB-->GBL???

Foxy Out

[Rhodium]

Convenient Synthesis of gamma-Butyrolactone, J. Chem. Educ. 75-84 (1998)

They reflux sodium GHB with acid and extract the solution to get GBL.

http://rhodium.lycaeum.org

[foxy2]

Thank You Very Much Rhodium
Hey
Cheapskate, Q981?, and other GHB researchers
This would be a great clean up method

1. Form GBL
2. Extract with CH2Cl2, and wash with slightly acidic H2O
3. Convert to GHB with basic H2O
4. Ensure complete separation to H2O
5. Separate aqueous and hydrophobic phases
6. Wash H2O/GHB mixture with hydrophobic
  (experiment to see what takes the most crap out)
7. Repeat or Isolate product when purity is up to
   your specifications

It reminds me of an Acid/Base extraction only a little
trickier, but im sure cheapskate is up to the task
Well thats my contribution for the week  

Foxy Out

[Rhodium]

Convenient Synthesis of a Lactone, ?-Butyrolactone
Richard E. Bozak, J. Knittel, and Ronald J. Hicks
Journal of Chemical Education 75(1), 84 (1998)

Lactones are cyclic esters. They are claimed to be most stable when the ring is either 5- or 6-membered¹. While lactones are usually ignored in first-year organic chemistry, this experiment shows that they might have some pedagogical virtues. The starting material in this student-oriented microscale experiment is a commercially available salt². Also, the boiling point is noteworthy in that the open-chain form, ethyl acetate, has a boiling point of 77°C, whereas the ring form boils at 206°C! One might ideally end this experiment with a vacuum distillation³. In our hands, the KBr pellet IR spectrum had its C=O stretch at 1763 cm^-1.

Procedure

Place 1.5 g (11.9 mmol) of ?-hydroxybutyric acid sodium salt⁴ into a 5-mL conical vial that contains a spin vane. Carefully add 1.5 mL of 9 M H₂SO₄, attach an air condenser, and reflux the mixture for 15 minutes. Upon cooling, crystals of sodium sulfate may form.

Extract the reaction mixture with 1.5 mL of CH₂Cl₂. Shake well with frequent venting. Allow the phases to separate and transfer the upper layer, using a filter-tip pipet, to a glass centrifuge tube. Repeat the extraction with a second 1.5 mL portion of CH₂Cl₂ and transfer the upper layer to the centrifuge tube as before. Dry the organic phase in the corked centrifuge tube with three microscoopula tips (about 0.25 g) of anhydrous Na₂SO₄ (at least 15 minutes).

Transfer the dried CH₂Cl₂/lactone extract, using a clean filter-tip pipet, to a pre-weighed vial. Evaporate the CH₂Cl₂ using a hot-plate and a gentle stream of N₂ until the weight of the vial and liquid remains constant, then re-weigh. Determine the percent yield in the usual manner, obtain an IR spectrum, and compare it to an authentic IR spectrum of ?-butyrolactone.

Literature Cited

1. Roberts, J. D.; Caserio, M. C. Basic Principles of Organic Chemistry; Benjamin: Menlo Park, CA, 1964; p 529.
2. Catalog Handbook of Fine Chemicals; Aldrich Chemical Company: Milwaukee, WI, 1996–1997; p 813.
3. See, for example: Pavia, D. L.; Lampman, G. M.; Kriz, G. S.; Engel, R. G. Organic Laboratory Techniques, A Microscale Approach; Saunders College: Orlando, FL, 1995; pp 677–693.
4. In biology-oriented areas, this is referred to as “GHB”; see, for instance, Laborit, H.

Int. J. Neuropharmacol. 3, 433-452 (1964)

(https://www.thevespiary.org/rhodium/Rhodium/pdf/ghb.review.laborit.pdf)

[Aurelius]

Why take it that direction when it's already in the salt form?

[Novice]

I believe the intention was to purify "ghetto GHB" and a convenient way to do it is to convert the salt into the lactone and distill it. Perhaps?

[Nicodem]

Perhaps it was with an educational intent. A paper from the Journal of Chemical Education might bee educational for bees too even though the (bee)wanted product is actually the precursor and the precursor a (bee)wanted product.

[Chimitant]

Maybe this bee just wants to be on the save side ? After all, GHB is something you´re not suppose to have   . GBL gives no problem (at least in Europe).

[Raver71]

[armageddon]

Convert GHB*Na to GBL by refluxing in dilute mineral acid, concentrate to 1/2 volume under vacuum, extract remainder at least five times with twice its amount of CHCl2, combine extracts, dry, remove solvent in a rotovap and vacuum distill the remaining GBL, then follow the usual procedure to get GHB*X again...

(outstanding purity guaranteed!   )

Greetz A