Technology Process of 3-amino-5-(2,4,6-trichloro-phenyl)-1,3-dihydro-benzo[e][1,4]diazepin-2-one hydrochloride
There total 8 articles about 3-amino-5-(2,4,6-trichloro-phenyl)-1,3-dihydro-benzo[e][1,4]diazepin-2-one hydrochloride which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
[1-(4-methoxy-benzyl)-2-oxo-5-(2,4,6-trichloro-phenyl)-2,3-dihydro-1H-benzo[e][1,4]diazepin-3-yl]-carbamic acid tert-butyl ester;
With
aluminum (III) chloride;
In
methoxybenzene;
at 70 ℃;
for 4h;
With
hydrogenchloride;
In
dichloromethane;
for 2h;
- Guidance literature:
-
Multi-step reaction with 6 steps
1.1: acetic acid / 24 h / 92 °C / Industry scale; Inert atmosphere
2.1: N,N-dimethyl-aniline; phosphorus trichloride / toluene / 16 h / 110 °C / Industry scale; Inert atmosphere
2.2: 25 °C / pH > 12
3.1: 2,4,6-Triisopropylbenzenesulfonyl azide; potassium tert-butylate / 2-methyltetrahydrofuran / 2.5 h / 40 - 50 °C / Inert atmosphere; 3 ? molecular sieve
3.2: 36 h / -20 - 30 °C / pH > 12
4.1: hydrogen / platinum(IV) oxide / 1,4-dioxane / 3 h / 7500.75 Torr / Industry scale; Autoclave
5.1: potassium carbonate; silver carbonate / tetrakis(triphenylphosphine) palladium(0) / tetrahydrofuran / 72 h / Reflux
6.1: aluminum (III) chloride / methoxybenzene / 4 h / 70 °C
6.2: 2 h
With
aluminum (III) chloride; 2,4,6-Triisopropylbenzenesulfonyl azide; potassium tert-butylate; hydrogen; potassium carbonate; acetic acid; N,N-dimethyl-aniline; silver carbonate; phosphorus trichloride;
platinum(IV) oxide; tetrakis(triphenylphosphine) palladium(0);
In
tetrahydrofuran; 2-methyltetrahydrofuran; 1,4-dioxane; methoxybenzene; toluene;
- Guidance literature:
-
Multi-step reaction with 8 steps
1.1: acetic acid / dichloromethane / 0.5 h / 40 °C / Industry scale; Inert atmosphere
1.2: 5 °C
2.1: tetrahydrofuran / 16 h / 15 - 20 °C
3.1: acetic acid / 24 h / 92 °C / Industry scale; Inert atmosphere
4.1: N,N-dimethyl-aniline; phosphorus trichloride / toluene / 16 h / 110 °C / Industry scale; Inert atmosphere
4.2: 25 °C / pH > 12
5.1: 2,4,6-Triisopropylbenzenesulfonyl azide; potassium tert-butylate / 2-methyltetrahydrofuran / 2.5 h / 40 - 50 °C / Inert atmosphere; 3 ? molecular sieve
5.2: 36 h / -20 - 30 °C / pH > 12
6.1: hydrogen / platinum(IV) oxide / 1,4-dioxane / 3 h / 7500.75 Torr / Industry scale; Autoclave
7.1: potassium carbonate; silver carbonate / tetrakis(triphenylphosphine) palladium(0) / tetrahydrofuran / 72 h / Reflux
8.1: aluminum (III) chloride / methoxybenzene / 4 h / 70 °C
8.2: 2 h
With
aluminum (III) chloride; 2,4,6-Triisopropylbenzenesulfonyl azide; potassium tert-butylate; hydrogen; potassium carbonate; acetic acid; N,N-dimethyl-aniline; silver carbonate; phosphorus trichloride;
platinum(IV) oxide; tetrakis(triphenylphosphine) palladium(0);
In
tetrahydrofuran; 2-methyltetrahydrofuran; 1,4-dioxane; dichloromethane; methoxybenzene; toluene;