Technology Process of 9-chloro-2-({3-[3-(dimethylamino)propyl]-2-methoxyphenyl}amino)-5,7-dihydro-6H-pyrimido[5,4-d][1]benzazepin-6-one
There total 10 articles about 9-chloro-2-({3-[3-(dimethylamino)propyl]-2-methoxyphenyl}amino)-5,7-dihydro-6H-pyrimido[5,4-d][1]benzazepin-6-one which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
With
hydrogenchloride; palladium 10% on activated carbon; hydrogen;
In
tetrahydrofuran; 1,4-dioxane; water;
at 20 ℃;
for 1.5h;
under 760.051 Torr;
Inert atmosphere;
DOI:10.1021/jm2011172
- Guidance literature:
-
Multi-step reaction with 3 steps
1: copper(l) iodide; bis-triphenylphosphine-palladium(II) chloride; triethylamine / 70 °C / Inert atmosphere
2: tris-(dibenzylideneacetone)dipalladium(0); caesium carbonate; 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene / 1,4-dioxane / 100 °C / Inert atmosphere
3: hydrogenchloride; palladium 10% on activated carbon; hydrogen / tetrahydrofuran; 1,4-dioxane; water / 1.5 h / 20 °C / 760.05 Torr / Inert atmosphere
With
hydrogenchloride; bis-triphenylphosphine-palladium(II) chloride; tris-(dibenzylideneacetone)dipalladium(0); copper(l) iodide; palladium 10% on activated carbon; hydrogen; caesium carbonate; triethylamine; 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene;
In
tetrahydrofuran; 1,4-dioxane; water;
DOI:10.1021/jm2011172
- Guidance literature:
-
Multi-step reaction with 7 steps
1.1: dmap; N-ethyl-N,N-diisopropylamine / dichloromethane / 20 °C
2.1: potassium tert-butylate / tetrahydrofuran / 10 °C
2.2: 20 °C / pH 4
3.1: water / dimethyl sulfoxide / 150 °C / Cooling
3.2: 0 °C
4.1: tetrahydrofuran / 2 h / 60 °C / Inert atmosphere
5.1: potassium carbonate / ethanol / 75 °C
6.1: tris-(dibenzylideneacetone)dipalladium(0); caesium carbonate; 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene / 1,4-dioxane / 100 °C / Inert atmosphere
7.1: hydrogenchloride; palladium 10% on activated carbon; hydrogen / tetrahydrofuran; 1,4-dioxane; water / 1.5 h / 20 °C / 760.05 Torr / Inert atmosphere
With
hydrogenchloride; dmap; tris-(dibenzylideneacetone)dipalladium(0); palladium 10% on activated carbon; potassium tert-butylate; water; hydrogen; potassium carbonate; caesium carbonate; N-ethyl-N,N-diisopropylamine; 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene;
In
tetrahydrofuran; 1,4-dioxane; ethanol; dichloromethane; water; dimethyl sulfoxide;
2.1: Dieckmann reaction;
DOI:10.1021/jm2011172
