Technology Process of ((3S)-3-(((2R)-2-((1S)-2-amino-1-(cyclopropylmethyl)-2-oxoethyl)-5,5,5-trifluoropentanoyl)amino)-9-fluoro-2-oxo-5-phenyl-2,3-dihydro-1H-1,4-benzodiazepin-1-yl)methyl L-valinate
There total 20 articles about ((3S)-3-(((2R)-2-((1S)-2-amino-1-(cyclopropylmethyl)-2-oxoethyl)-5,5,5-trifluoropentanoyl)amino)-9-fluoro-2-oxo-5-phenyl-2,3-dihydro-1H-1,4-benzodiazepin-1-yl)methyl L-valinate which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
C37H45F4N5O7;
With
hydrogenchloride;
In
1,4-dioxane; dichloromethane;
at 0 - 20 ℃;
for 2h;
In
methanol; water; acetonitrile; trifluoroacetic acid;
Resolution of racemate;
- Guidance literature:
-
Multi-step reaction with 6 steps
1.1: oxalyl dichloride / N,N-dimethyl-formamide; tetrahydrofuran / 1.5 h / 0 °C
1.2: 20 °C
2.1: hydrogen bromide; acetic acid / 1.5 h / 20 °C
3.1: triethylamine; O-(benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborate / N,N-dimethyl-formamide / 1.5 h / 20 °C
4.1: trifluoroacetic acid / dichloromethane / 1.83 h / 20 °C
4.2: 8 - 20 °C
4.3: Lux-Cell4 / 40 °C / 75007.5 Torr / Supercritical conditions; liquid CO2
5.1: potassium carbonate / N,N-dimethyl-formamide / 0.17 h
5.2: 20 °C
6.1: hydrogenchloride / dichloromethane; 1,4-dioxane / 2 h / 0 - 20 °C
6.2: SunFire C18 / Resolution of racemate
With
hydrogenchloride; oxalyl dichloride; hydrogen bromide; potassium carbonate; O-(benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborate; acetic acid; triethylamine; trifluoroacetic acid;
In
tetrahydrofuran; 1,4-dioxane; dichloromethane; N,N-dimethyl-formamide;
- Guidance literature:
-
Multi-step reaction with 5 steps
1.1: hydrogen bromide; acetic acid / 1.5 h / 20 °C
2.1: triethylamine; O-(benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborate / N,N-dimethyl-formamide / 1.5 h / 20 °C
3.1: trifluoroacetic acid / dichloromethane / 1.83 h / 20 °C
3.2: 8 - 20 °C
3.3: Lux-Cell4 / 40 °C / 75007.5 Torr / Supercritical conditions; liquid CO2
4.1: potassium carbonate / N,N-dimethyl-formamide / 0.17 h
4.2: 20 °C
5.1: hydrogenchloride / dichloromethane; 1,4-dioxane / 2 h / 0 - 20 °C
5.2: SunFire C18 / Resolution of racemate
With
hydrogenchloride; hydrogen bromide; potassium carbonate; O-(benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborate; acetic acid; triethylamine; trifluoroacetic acid;
In
1,4-dioxane; dichloromethane; N,N-dimethyl-formamide;
