Ketamine methylamine question

[Sciencenutz]

Synthesis of 2-hydroxy-2-(2-chlorophenyl)-1-
cyclohexane-N-methylimine (V)
In a 250 mL round bottom flask, 2-(2-chlorophenyl)-2-hy-
droxycyclohexane-1-one (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,
filtered and the solvent was evaporated by rotary evapora-
tor. Finally, purification of the product by a silica gel col-
umn chromatography (20:3 hexane/ethyl acetate) produced
2-hydroxy-2-(2-chlorophenyl)-1-cyclohexane-N-methylim-
ine as a white liquid (yield 91%).


My question is on scale up for 1kg of 2-(2-chlorophenyl)-2-hydroxycyclohexane-1-one and 183g k2C03 how many ml of liquid methylamine would you use?

 

[btcboss2022]

Synthesis of 2-hydroxy-2-(2-chlorophenyl)-1-
cyclohexane-N-methylimine (V)
In a 250 mL round bottom flask, 2-(2-chlorophenyl)-2-hy-
droxycyclohexane-1-one (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,
filtered and the solvent was evaporated by rotary evapora-
tor. Finally, purification of the product by a silica gel col-
umn chromatography (20:3 hexane/ethyl acetate) produced
2-hydroxy-2-(2-chlorophenyl)-1-cyclohexane-N-methylim-
ine as a white liquid (yield 91%).


My question is on scale up for 1kg of 2-(2-chlorophenyl)-2-hydroxycyclohexane-1-one and 183g k2C03 how many ml of liquid methylamine would you use?

SciencenutzDepend on your methylamine concentration but I guess that for pure freebase is 4,46L from this data you can make proportions.

 

[Sciencenutz]

Well synthesis says to do 40% w/w so would it just be 1mol of hydroxy to 1mol of methylaminr with a bit of excess?

 

[btcboss2022]

Well synthesis says to do 40% w/w so would it just be 1mol of hydroxy to 1mol of methylaminr with a bit of excess?

Sciencenutz4.46L of 40% solution then.

 

[Sciencenutz]

4.46L of 40% solution then.

btcboss2022Yes so 600g methanol and 500g methylamine and 250g lye should be around 40% right?

 

[btcboss2022]

Yes so 600g methanol and 500g methylamine and 250g lye should be around 40% right?

SciencenutzFrom Methylamine HCL you must trap the gas in cold methanol. To know the amount of Methylamine absorved you must weight the methanol. Not easy process.

 

[Davidrobinson]

Where are you getting 1Kg of
chlorophenyl)-2-hy-
droxycyclohexane-1-one

 

[btcboss2022]

Where are you getting 1Kg of
chlorophenyl)-2-hy-
droxycyclohexane-1-one

oscar412Is commercially available but price is to high not profitable deal for final stuff. I mean is cheaper to buy directly the final stuff.

 

[Davidrobinson]

Do You have conversion for the nitro to this^^