Bdo to gbl

[Sciencenutz]

How do you look up references for synthesis I'm trying to do bdo to gbl and have this but when I look up I can't find the synthesis?

Reaction 5 (Sodium bromite)​

Reagent: sodium bromite
Solvent: H2O acetic acid
Time: 10 hours
Other Conditions: Ambient temperature
Yield 92%
Ref. 1 5666548; Journal; Kageyama, Toshifumi; Kawahara, Shuji; Kitamura, Kohji; Ueno, Yoshio; Okawara, Makoto; CMLTAG; Chem.Lett.; EN; 1983; 1097-1100;

 

[UWe9o12jkied91d]

But why? 1,4-butanediol is already a prodrug for GHB
Also what else do you need? Everything is here

 

[UWe9o12jkied91d]

anyways, here you go

https://www.journal.csj.jp/doi/pdf/10.1246/cl.1983.1097

 

[Sciencenutz]

Where I'm from people are in need of gbl and ghb as bdo isn't acceptable. I have been having issues with bdo to gbl with copper chromite as for some reason on my heating mantle I can't get the temp to 200c...it stops at around 190c and then slowly drops...even though my mantle temp can easily get it to over 200c it just doesn't seem to want to go higher

 

[UWe9o12jkied91d]

They smell very simillar, the smell is weak so not even as discernable, with very simillar effects for GBL atleast.

 

[Sciencenutz]

Do you have any experience running this reaction with copper chromite?

 

[UWe9o12jkied91d]

No

 

[Sciencenutz]

Also how did you search that ref # I have a few others I'm interested in

 

[UWe9o12jkied91d]

I’ll try to find the rest if you provide them, reaserch is what I do for a living, don’t feel like writing a guide rn

 

[Sciencenutz]

Reagent: NaBrO2*3H20, Al2O3
Solvent: CH2Cl2
Other Conditions: Ambient temperature
Yield 92%
Ref. 1 5895926; Journal; Morimoto, Takashi; Hirano, Masao; Iwasaki, Keiko; Ishikawa, Takashi; CMLTAG; Chem.Lett.; EN; 1; 1994; 53-54;

 

[UWe9o12jkied91d]

Sci-Hub | Oxidation of Diols with Sodium Bromite Trihydrate in Organic Solvents in the Presence of Alumina. Chemistry Letters, 23(1), 53–54 | 10.1246/cl.1994.53

 

[Sciencenutz]

Have you done bdo to gbl with copper chromite at 200c before? I'm having trouble converting it I can only get to 190c and temp drops around 13c and hydrogen occurs boil for 3 4 hours then distill but when put in freezer it goes solid any ideas?

 

[Alkahest]

Reflux longer. Check periodically the evolution of hydrogen by attaching a balloon or something to the reflux condenser. Ignite it to verify. You will know that it has gone to completion when the reaction mixture is cooled and it has the consistency close to that of water. Also, consider using other copper catalysts, copper chromite is toxic, particularly devastating to aquatic life, don't pour down the sink. You should spend time to properly purify the end product.