Technology Process of 2-(3-(5-(1,5-dimethyl-1H-pyrazol-3-ylamino)-1-methyl-6-oxo-1,6-dihydropyridin-3-yl)-2-(hydroxymethyl)phenyl)-3,4,6,7,8,9-hexahydropyrazino[1,2-a]indol-1(2H)-one
There total 14 articles about 2-(3-(5-(1,5-dimethyl-1H-pyrazol-3-ylamino)-1-methyl-6-oxo-1,6-dihydropyridin-3-yl)-2-(hydroxymethyl)phenyl)-3,4,6,7,8,9-hexahydropyrazino[1,2-a]indol-1(2H)-one which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
With
water; lithium hydroxide;
In
tetrahydrofuran; isopropyl alcohol;
at 30 ℃;
for 2h;
- Guidance literature:
-
Multi-step reaction with 6 steps
1: N-Bromosuccinimide / 2,2'-azobis(isobutyronitrile) / tetrachloromethane / 14 h / 80 °C / Inert atmosphere
2: N,N-dimethyl-formamide / 14 h / 20 °C / Inert atmosphere
3: caesium carbonate / copper(l) iodide; N,N`-dimethylethylenediamine / 1,4-dioxane / 16 h / 95 °C / Inert atmosphere; sealed tube
4: potassium acetate / dichloro(1,1'-bis(diphenylphosphanyl)ferrocene)palladium(II)*CH2Cl2 / 1,4-dioxane / 95 °C / Inert atmosphere
5: potassium phosphate; sodium acetate / (1,1'-bis(diphenylphosphino)ferrocene)palladium(II) dichloride / acetonitrile; water / 15 h / 110 °C / Inert atmosphere
6: water; lithium hydroxide / isopropyl alcohol; tetrahydrofuran / 2 h / 30 °C
With
potassium phosphate; N-Bromosuccinimide; water; potassium acetate; sodium acetate; caesium carbonate; lithium hydroxide;
(1,1'-bis(diphenylphosphino)ferrocene)palladium(II) dichloride; copper(l) iodide; dichloro(1,1'-bis(diphenylphosphanyl)ferrocene)palladium(II)*CH2Cl2; 2,2'-azobis(isobutyronitrile); N,N`-dimethylethylenediamine;
In
tetrahydrofuran; 1,4-dioxane; tetrachloromethane; water; N,N-dimethyl-formamide; isopropyl alcohol; acetonitrile;
- Guidance literature:
-
Multi-step reaction with 4 steps
1.1: caesium carbonate / 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene; tris-(dibenzylideneacetone)dipalladium(0) / 1,4-dioxane / 48 h / 115 °C / Inert atmosphere; sealed tube
2.1: sodium hydride / N,N-dimethyl-formamide; mineral oil / 0.5 h / Inert atmosphere
2.2: 2 h / Inert atmosphere
3.1: potassium phosphate; sodium acetate / (1,1'-bis(diphenylphosphino)ferrocene)palladium(II) dichloride / acetonitrile; water / 15 h / 110 °C / Inert atmosphere
4.1: water; lithium hydroxide / isopropyl alcohol; tetrahydrofuran / 2 h / 30 °C
With
potassium phosphate; water; sodium acetate; sodium hydride; caesium carbonate; lithium hydroxide;
(1,1'-bis(diphenylphosphino)ferrocene)palladium(II) dichloride; tris-(dibenzylideneacetone)dipalladium(0); 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene;
In
tetrahydrofuran; 1,4-dioxane; water; N,N-dimethyl-formamide; isopropyl alcohol; acetonitrile; mineral oil;