Technology Process of (3S,5S)-3-amino-5-(2,3-difluorophenyl)-1-(2,2,2-trifluoroethyl)piperidin-2-one hydrochloride
There total 7 articles about (3S,5S)-3-amino-5-(2,3-difluorophenyl)-1-(2,2,2-trifluoroethyl)piperidin-2-one hydrochloride which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
With
hydrogenchloride;
In
ethyl acetate;
at 0 ℃;
for 0.5h;
- Guidance literature:
-
Multi-step reaction with 6 steps
1.1: potassium hydroxide; hydroquinone / methanol / 16 h / 160 °C
2.1: hydrogen; ammonia / Raney nickel / ethanol; water / 18 h / 760.05 Torr
3.1: lithium hexamethyldisilazane / 1-methyl-pyrrolidin-2-one; tetrahydrofuran / 0.33 h / 0 - 5 °C
3.2: 3 h / 0 - 20 °C
4.1: lithium hexamethyldisilazane / tetrahydrofuran / 0.5 h / -78 - -65 °C
4.2: 0.75 h / -78 - 65 °C
4.3: -78 - 20 °C
5.1: hydrogen / palladium 10% on activated carbon / ethanol / 18 h / 760.05 Torr
5.2: Chiralcel.(R). AD column / Resolution of racemate
6.1: hydrogenchloride / ethyl acetate / 0.5 h / 0 °C
With
hydrogenchloride; ammonia; hydrogen; hydroquinone; potassium hydroxide; lithium hexamethyldisilazane;
palladium 10% on activated carbon;
In
tetrahydrofuran; 1-methyl-pyrrolidin-2-one; methanol; ethanol; water; ethyl acetate;
- Guidance literature:
-
Multi-step reaction with 5 steps
1.1: hydrogen; ammonia / Raney nickel / ethanol; water / 18 h / 760.05 Torr
2.1: lithium hexamethyldisilazane / 1-methyl-pyrrolidin-2-one; tetrahydrofuran / 0.33 h / 0 - 5 °C
2.2: 3 h / 0 - 20 °C
3.1: lithium hexamethyldisilazane / tetrahydrofuran / 0.5 h / -78 - -65 °C
3.2: 0.75 h / -78 - 65 °C
3.3: -78 - 20 °C
4.1: hydrogen / palladium 10% on activated carbon / ethanol / 18 h / 760.05 Torr
4.2: Chiralcel.(R). AD column / Resolution of racemate
5.1: hydrogenchloride / ethyl acetate / 0.5 h / 0 °C
With
hydrogenchloride; ammonia; hydrogen; lithium hexamethyldisilazane;
palladium 10% on activated carbon;
In
tetrahydrofuran; 1-methyl-pyrrolidin-2-one; ethanol; water; ethyl acetate;