Technology Process of 1-[4-(7,9-difluoro-6H-pyrrolo[1,2-a][1,4]benzodiazepin-4-yl)phenyl]ethanone
There total 7 articles about 1-[4-(7,9-difluoro-6H-pyrrolo[1,2-a][1,4]benzodiazepin-4-yl)phenyl]ethanone which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
Multi-step reaction with 8 steps
1.1: hydrogenchloride; hydroxylamine hydrochloride; sodium sulfate / water / 1 h / Reflux
2.1: sulfuric acid / 2 h / 50 - 100 °C
2.2: 0 - 20 °C
2.3: pH 1
3.1: pyridine hydrochloride / 1,4-dioxane / Reflux
4.1: benzotriazol-1-ol; ammonium hydroxide; 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride / N,N-dimethyl-formamide
5.1: dimethylsulfide borane complex / tetrahydrofuran / Inert atmosphere; Reflux
5.2: 0.5 h / Reflux
6.1: ethanol / 4 h / Reflux
6.2: HPLC
7.1: sodium hydrogencarbonate
8.1: ammonium hydroxide / dichloromethane
8.2: 48 h / 20 °C
With
hydrogenchloride; dimethylsulfide borane complex; sulfuric acid; hydroxylamine hydrochloride; pyridine hydrochloride; sodium hydrogencarbonate; benzotriazol-1-ol; ammonium hydroxide; sodium sulfate; 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride;
In
tetrahydrofuran; 1,4-dioxane; ethanol; dichloromethane; water; N,N-dimethyl-formamide;
- Guidance literature:
-
Multi-step reaction with 6 steps
1.1: pyridine hydrochloride / 1,4-dioxane / Reflux
2.1: benzotriazol-1-ol; ammonium hydroxide; 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride / N,N-dimethyl-formamide
3.1: dimethylsulfide borane complex / tetrahydrofuran / Inert atmosphere; Reflux
3.2: 0.5 h / Reflux
4.1: ethanol / 4 h / Reflux
4.2: HPLC
5.1: sodium hydrogencarbonate
6.1: ammonium hydroxide / dichloromethane
6.2: 48 h / 20 °C
With
dimethylsulfide borane complex; pyridine hydrochloride; sodium hydrogencarbonate; benzotriazol-1-ol; ammonium hydroxide; 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride;
In
tetrahydrofuran; 1,4-dioxane; ethanol; dichloromethane; N,N-dimethyl-formamide;
- Guidance literature:
-
Multi-step reaction with 7 steps
1.1: sulfuric acid / 2 h / 50 - 100 °C
1.2: 0 - 20 °C
1.3: pH 1
2.1: pyridine hydrochloride / 1,4-dioxane / Reflux
3.1: benzotriazol-1-ol; ammonium hydroxide; 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride / N,N-dimethyl-formamide
4.1: dimethylsulfide borane complex / tetrahydrofuran / Inert atmosphere; Reflux
4.2: 0.5 h / Reflux
5.1: ethanol / 4 h / Reflux
5.2: HPLC
6.1: sodium hydrogencarbonate
7.1: ammonium hydroxide / dichloromethane
7.2: 48 h / 20 °C
With
dimethylsulfide borane complex; sulfuric acid; pyridine hydrochloride; sodium hydrogencarbonate; benzotriazol-1-ol; ammonium hydroxide; 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride;
In
tetrahydrofuran; 1,4-dioxane; ethanol; dichloromethane; N,N-dimethyl-formamide;
