Technology Process of 2-[(4-{[2-(3,4-dichlorophenyl)ethyl]amino}-1-piperidinyl)methyl]-1,2-dihydro-3H,8H-2a,5,8a-triazaacenaphthylene-3,8-dione
There total 11 articles about 2-[(4-{[2-(3,4-dichlorophenyl)ethyl]amino}-1-piperidinyl)methyl]-1,2-dihydro-3H,8H-2a,5,8a-triazaacenaphthylene-3,8-dione which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
2-[(4-amino-1-piperidinyl)methyl]-1,2-dihydro-3H,8H-2a,5,8a-triazaacenaphthylene-3,8-dione; 2-(3,4-dichlorophenyl)ethyl methanesulfonate;
With
potassium carbonate;
In
acetonitrile;
at 60 ℃;
Reflux;
sodium iodide;
In
acetonitrile;
at 20 ℃;
- Guidance literature:
-
Multi-step reaction with 11 steps
1.1: toluene-4-sulfonic acid / 20 °C / Inert atmosphere
1.2: 0.33 h
2.1: hydrogen / palladium 10% on activated carbon / 1,4-dioxane; water / 18 h / 20 °C / 760.05 Torr
3.1: potassium carbonate / N,N-dimethyl-formamide / 20 °C / Inert atmosphere
4.1: sodium hydride / tetrahydrofuran; mineral oil / 0 - 20 °C / Inert atmosphere
4.2: 0 - 20 °C
5.1: manganese(IV) oxide / dichloromethane / 2 h / 20 °C
6.1: hydrogenchloride; water / tetrahydrofuran / 1 h / 20 °C
6.2: pH ~ 8
7.1: triethylamine / chloroform / 4.5 h / Reflux; Inert atmosphere
8.1: pyridine / acetonitrile / 50 - 90 °C / Reflux; Inert atmosphere
9.1: hydrogenchloride / 1,4-dioxane; dichloromethane / 20 °C
10.1: ammonia / methanol; water
11.1: potassium carbonate / acetonitrile / 60 °C / Reflux
11.2: 20 °C
With
pyridine; hydrogenchloride; manganese(IV) oxide; ammonia; water; hydrogen; sodium hydride; potassium carbonate; toluene-4-sulfonic acid; triethylamine;
palladium 10% on activated carbon;
In
tetrahydrofuran; 1,4-dioxane; methanol; dichloromethane; chloroform; water; N,N-dimethyl-formamide; acetonitrile; mineral oil;
- Guidance literature:
-
Multi-step reaction with 12 steps
1.1: ethanol / 3 h / Inert atmosphere; Reflux
2.1: toluene-4-sulfonic acid / 20 °C / Inert atmosphere
2.2: 0.33 h
3.1: hydrogen / palladium 10% on activated carbon / 1,4-dioxane; water / 18 h / 20 °C / 760.05 Torr
4.1: potassium carbonate / N,N-dimethyl-formamide / 20 °C / Inert atmosphere
5.1: sodium hydride / tetrahydrofuran; mineral oil / 0 - 20 °C / Inert atmosphere
5.2: 0 - 20 °C
6.1: manganese(IV) oxide / dichloromethane / 2 h / 20 °C
7.1: hydrogenchloride; water / tetrahydrofuran / 1 h / 20 °C
7.2: pH ~ 8
8.1: triethylamine / chloroform / 4.5 h / Reflux; Inert atmosphere
9.1: pyridine / acetonitrile / 50 - 90 °C / Reflux; Inert atmosphere
10.1: hydrogenchloride / 1,4-dioxane; dichloromethane / 20 °C
11.1: ammonia / methanol; water
12.1: potassium carbonate / acetonitrile / 60 °C / Reflux
12.2: 20 °C
With
pyridine; hydrogenchloride; manganese(IV) oxide; ammonia; water; hydrogen; sodium hydride; potassium carbonate; toluene-4-sulfonic acid; triethylamine;
palladium 10% on activated carbon;
In
tetrahydrofuran; 1,4-dioxane; methanol; ethanol; dichloromethane; chloroform; water; N,N-dimethyl-formamide; acetonitrile; mineral oil;