Author Topic: ketamine synthesis from Hydroxylimine  (Read 2248 times)

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bimmer

  • Guest
ketamine synthesis from Hydroxylimine
« on: May 24, 2004, 04:45:00 AM »
Ok, since ketamine freebase is regulated in china now like ketamine hcl, all I have available to me is Hydroxylimine and Hydroxylimine HCL. I have converted freebase to ketamine hcl, but never touched Hydroxylimine.  I have conversions given to me from china but would like to know if anyone has simpler conversions. Or perhaps somthing a little easier to understand. Any help would be apreciated. Here is what I currently have-
Conversion process from Hydroxylimine to freebase

1.   Certain weight of Hydroxylimine, assay 95% min, add in 1.5 times weight of Ethyl Benzoate, heat to 40  50 C to dissolve Hydroxylimine basically.
2.   Cool the solution to 20 C, keep stiring and add in HCl vapor till pH 1.5  2.0.
3.   Heat the solution to 180 C, hold on 30 minutes.
4.   Cool the solution to 0 C, hold on 2 hours, filter or centrifugate to separate liquid and get dry compound.
5.   Dry the compound at 80 C for 6 hours, now appears brown colour.
6.   Add in 10 times weight of water, heat the solution to 70 C, add in 5% weight of active carbon, stir up 30 minutes.
7.   Filter to separate carbon, add in active carbon as the above and filter again, totally three times of adding in carbon and filtering, each time the effective compound in container must be cleaned up by water and filtered to ensure collecting everthing. The final filterd liquid should be yellowish colour.
8.   Cool the liquid to 20 C, add in 10% NaOH solution, till pH 8  9, now obtain freebase lye.  The flake caustic (NaOH) must be in high grade and dissolved by distilled water.
9.   Centrifugate the lye at 20 C, dried by heating at about 60 C, start from 50 C and gradually up to 80 C for 24 hours. It takes long time drying due to low Melting point of freebase.

Notice:
1.   To heat the solution to 180 C, a porcelain enamel electrical heating reactor should be used. The reactor is jacketed, the electrical heated oil in between the jacketed walls. The process of heating must be in a short time (1  2 hours). So the reactor should be with higher power, not less than 15 KW, and a good insulatiing layer.
2.   For a better reaction, the input of one batch should not be larger than 30 kgs. The reactor size is 100 litre.
3.   Ethyl Benzoate has strong odor.

Molecular Structure of Hydroxylimide and freebase:

                     

The yield of freebase from Hydroxylimide is 80%, of k hcl 88%.

speck1

  • Guest
eaisier way
« Reply #1 on: August 19, 2004, 08:13:00 AM »
there is a eaisier way that takes 8  hrs just email me at billbaker67@hotmail.com
latest addition (08-19-04):