G.Patton
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i can find nobody that sell this chemical?
what? You can't find? Open google or so and put "2-chlorophenyl hydroxy cyclohexanone buy"
i can find nobody that sell this chemical?
what? You can't find? Open google or so and put "2-chlorophenyl hydroxy cyclohexanone buy"
29.0g of above bromoketone is dissolved in 50 ml of liquid methylamine freebase. Benzene may also be used as solvent. After one hour, the excess liquid methylamine is allowed to evaporate, although increasing the reaction time to 4-5 days may increase yield. The residue is then dissolved in pentane and filtered. The solvent is evaporated to yield 1-hydroxy-cyclopentyl-(o-chlorophenyl)-ketone N-methylimine, mp 62 C (yield ~84%).
The final step is a thermal rearrangement, and gives almost quantitative yield after 180 C for 30 min. An alternative to the use of decalin as solvent in this step is to use a pressure bomb.
2.0 g of the preceeding N-methylimine is dissolved in 15 ml of decalin and refluxed for 2.5 h. After evaporation of the solvent under reduced pressure, the residue is extracted with dilute hydrochloric acid, the solution treated with decolorizing charcoal, and the resulting acidic solution is made basic. The liberated product, 2-methylamino-2-(o-chlorophenyl)-cyclohexanone (Ketamine), after recrystallization from pentane-ether, has a mp of 92-93C. The hydrochloride has a mp of 262-263 C.
As with PCE, the freebase is too caustic to be smoked, and must be converted into the HCl salt in order to be consumed in this manner.
In my opinion is easier this from :
1-hydroxycyclopentyl-(o-chlorophenyl)-ketone-N-methylimine
2-Methylamino-2-(o-chlorophenyl)-cyclohexanone (Ketamine)
has anyone found synthesis route for 2-(2-Chlorophenyl)-2-nitrocyclohexanone to ketamine?
3. CyclopentanoneAs I found recently, this can bee simplified yet more, by forming benzamides in situ from the corresponding acid and urea..but since this is a very good route to subst’d benzaldehydes from benzoic acids, I’ll post it later separately.
4. Aluminium isopropoxideNotes:
- Ca(OH)2 may bee substituted for Ba(OH)2 without much loss in the yield.
- if one is to use pre-made Ca or Ba adipinate, no temp control is necessary.
8. o-Chlorophenyl cyclopentyl ketoneNotes on the possible usage of Zn-organics:
".. Nitriles are not bad as electrophiles, so it is possible that despite smaller reactivity of ZnR2 compounds, they would work equally well here - esp. if the rxn conditions are made harsher (gentle reflux instead of RT?).
What one CAN say for sure-is that the rxn with ZnR2 will go just fine if one is to use o-chlorobenzoyl chloride instead of benzonitrile. Haloanhydrides generally are the best species for coupling with metalloorganics.
Bis-dicyclopentyl zinc is conveniently made from the corresponding bromide, no need to make iodide here. And o-chlorobenzoyl chloride can bee easily prepared from o-chlorobenzoic acid (obtained in Step 1) and PCl5 or some such."
Synthesis of 2-hydroxy-2-(2-chlorophenyl)-1-cyclohexane-N-methylimine (2)
In a 250 mL round bottom flask, 2-(2-chlorophenyl)-2-hydroxycyclohexane-1-one (1) (11.20 g, 50 mmol), K2CO3 (2.05 g, 15 mmol) and 50 mL methylamine were poured, and kept in dark and stirred for 48 h at room temperature. Further, the reaction mixture was washed with dry THF (3 x 100 mL) in separatory funnel, filtered and the solvent was evaporated by rotary evaporator. Finally, purification of the product by a silica gel column chromatography (20:3 hexane/ethyl acetate) produced 2-hydroxy-2-(2-chlorophenyl)-1-cyclohexane-N-methylimine (2) as a white liquid (yield 91 %).
Mind if I ask, what kind of Methylamine is used here? 40% water solution? Or pure liquid MeNH2?
Thanks!
CAS 1823362-29-3 is not avaible anymore so it shouldnt matter.
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