Technology Process of tert-butyl [1-(4-{2-[4-(pyrrolidin-1-ylcarbonyl)phenyl]-9H-imidazo[1,2-d]pyrido[2,3-b][1,4]benzodiazepin-3-yl}phenyl)cyclobutyl]carbamate
There total 9 articles about tert-butyl [1-(4-{2-[4-(pyrrolidin-1-ylcarbonyl)phenyl]-9H-imidazo[1,2-d]pyrido[2,3-b][1,4]benzodiazepin-3-yl}phenyl)cyclobutyl]carbamate which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
With
1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride;
In
dichloromethane;
at 20 ℃;
for 24h;
- Guidance literature:
-
Multi-step reaction with 9 steps
1: Lawessons reagent; pyridine / 18 h / 100 °C
2: 1 h / 95 °C
3: acetic acid / 13 h / 105 °C
4: N-Bromosuccinimide / tetrahydrofuran / 2 h / 0 - 20 °C
5: tetrakis(triphenylphosphine) palladium(0); sodium hydrogencarbonate / ethanol; water; toluene / 15 h / Reflux
6: N-chloro-succinimide / chloroform / 22 h / Reflux
7: bis(di-tert-?butyl(4-?dimethylaminophenyl)?phosphine)?dichloropalladium(II); sodium carbonate / water; N,N-dimethyl-formamide / 1 h / 160 °C / Microwave irradiation
8: hydrogen / palladium 10% on activated carbon / methanol / 24.5 h / 50 °C
9: 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride / dichloromethane / 24 h / 20 °C
With
Lawessons reagent; pyridine; N-chloro-succinimide; N-Bromosuccinimide; tetrakis(triphenylphosphine) palladium(0); bis(di-tert-?butyl(4-?dimethylaminophenyl)?phosphine)?dichloropalladium(II); hydrogen; sodium hydrogencarbonate; sodium carbonate; acetic acid; 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride;
palladium 10% on activated carbon;
In
tetrahydrofuran; methanol; ethanol; dichloromethane; chloroform; water; N,N-dimethyl-formamide; toluene;
- Guidance literature:
-
Multi-step reaction with 8 steps
1: 1 h / 95 °C
2: acetic acid / 13 h / 105 °C
3: N-Bromosuccinimide / tetrahydrofuran / 2 h / 0 - 20 °C
4: tetrakis(triphenylphosphine) palladium(0); sodium hydrogencarbonate / ethanol; water; toluene / 15 h / Reflux
5: N-chloro-succinimide / chloroform / 22 h / Reflux
6: bis(di-tert-?butyl(4-?dimethylaminophenyl)?phosphine)?dichloropalladium(II); sodium carbonate / water; N,N-dimethyl-formamide / 1 h / 160 °C / Microwave irradiation
7: hydrogen / palladium 10% on activated carbon / methanol / 24.5 h / 50 °C
8: 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride / dichloromethane / 24 h / 20 °C
With
N-chloro-succinimide; N-Bromosuccinimide; tetrakis(triphenylphosphine) palladium(0); bis(di-tert-?butyl(4-?dimethylaminophenyl)?phosphine)?dichloropalladium(II); hydrogen; sodium hydrogencarbonate; sodium carbonate; acetic acid; 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride;
palladium 10% on activated carbon;
In
tetrahydrofuran; methanol; ethanol; dichloromethane; chloroform; water; N,N-dimethyl-formamide; toluene;