Technology Process of (4R)-4H-[1,2,4]triazolo[4,3-a][1,5]benzodiazepine, 5,6-dihydro-1,4-dimethyl-8-(pyrrolidine-1carbonyl)-6-(4-chloro-phenyl)
There total 7 articles about (4R)-4H-[1,2,4]triazolo[4,3-a][1,5]benzodiazepine, 5,6-dihydro-1,4-dimethyl-8-(pyrrolidine-1carbonyl)-6-(4-chloro-phenyl) which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
With
1,3-bis-(diphenylphosphino)propane; triethylamine;
palladium diacetate;
at 90 ℃;
for 12h;
- Guidance literature:
-
Multi-step reaction with 7 steps
1: ammonium chloride; iron / ethanol; water / 2 h / 60 °C
2: sodium / methanol / 0 - 20 °C
3: Lawessons reagent / tetrahydrofuran / 12 h / 80 °C
4: butan-1-ol / 12 h / 130 °C
5: caesium carbonate; dicyclohexyl-(2',6'-dimethoxybiphenyl-2-yl)-phosphane / tris-(dibenzylideneacetone)dipalladium(0) / toluene / 12 h / 110 °C / Inert atmosphere
6: Daicel AD-H / 38 °C / Resolution of racemate
7: triethylamine; 1,3-bis-(diphenylphosphino)propane / palladium diacetate / 12 h / 90 °C
With
dicyclohexyl-(2',6'-dimethoxybiphenyl-2-yl)-phosphane; Lawessons reagent; 1,3-bis-(diphenylphosphino)propane; sodium; iron; ammonium chloride; caesium carbonate; triethylamine;
tris-(dibenzylideneacetone)dipalladium(0); palladium diacetate;
In
tetrahydrofuran; methanol; ethanol; water; toluene; butan-1-ol;
- Guidance literature:
-
Multi-step reaction with 6 steps
1: sodium / methanol / 0 - 20 °C
2: Lawessons reagent / tetrahydrofuran / 12 h / 80 °C
3: butan-1-ol / 12 h / 130 °C
4: caesium carbonate; dicyclohexyl-(2',6'-dimethoxybiphenyl-2-yl)-phosphane / tris-(dibenzylideneacetone)dipalladium(0) / toluene / 12 h / 110 °C / Inert atmosphere
5: Daicel AD-H / 38 °C / Resolution of racemate
6: triethylamine; 1,3-bis-(diphenylphosphino)propane / palladium diacetate / 12 h / 90 °C
With
dicyclohexyl-(2',6'-dimethoxybiphenyl-2-yl)-phosphane; Lawessons reagent; 1,3-bis-(diphenylphosphino)propane; sodium; caesium carbonate; triethylamine;
tris-(dibenzylideneacetone)dipalladium(0); palladium diacetate;
In
tetrahydrofuran; methanol; toluene; butan-1-ol;