Technology Process of ethyl 7-chloro-5-(2-chlorophenyl)-1-isobutyl-2-oxo-2,3,4,5-tetrahydro-1H-1-benzazepine-3-acetate
There total 10 articles about ethyl 7-chloro-5-(2-chlorophenyl)-1-isobutyl-2-oxo-2,3,4,5-tetrahydro-1H-1-benzazepine-3-acetate which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
7-chloro-5-(2-chlorophenyl)-1-isobutyl-1,3,4,5-tetrahydro-2H-1-benzazepin-2-one;
With
lithium diisopropyl amide;
In
tetrahydrofuran; hexane;
at 0 ℃;
for 0.25h;
ethyl iodoacetae;
In
tetrahydrofuran; hexane;
at -78 - 0 ℃;
for 1.25h;
DOI:10.1016/S0968-0896(01)00289-9
- Guidance literature:
-
Multi-step reaction with 9 steps
1.1: H2 / 10 percent Pd-C / ethyl acetate / atmospheric pressure
1.2: 8.0 g / p-TsOH*H2O / Heating
2.1: aq. NaOH / ethanol / 1 h
3.1: SOCl2; DMF / toluene
4.1: 4.5 g / AlCl3 / 1,2-dichloro-ethane / 1 h / 20 °C
5.1: 82 percent / NH2OH*HCl; AcONa / H2O; ethanol / 2 h / Heating
6.1: 63 percent / polyphosphoric acid / 0.33 h / 120 °C
7.1: 89 percent / NaH / dimethylformamide / 4 h / 20 °C
8.1: 80 percent / N-chlorosuccinimide / dimethylformamide / 7 h / 70 °C
9.1: LDA / hexane; tetrahydrofuran / 0.25 h / 0 °C
9.2: 16 percent / hexane; tetrahydrofuran / 1.25 h / -78 - 0 °C
With
sodium hydroxide; N-chloro-succinimide; aluminium trichloride; thionyl chloride; PPA; hydroxylamine hydrochloride; hydrogen; sodium acetate; sodium hydride; N,N-dimethyl-formamide; lithium diisopropyl amide;
palladium on activated charcoal;
In
tetrahydrofuran; ethanol; hexane; water; ethyl acetate; 1,2-dichloro-ethane; N,N-dimethyl-formamide; toluene;
4.1: intramolecular Friedel-Crafts acylation / 6.1: Beckmann rearrangement;
DOI:10.1016/S0968-0896(01)00289-9
- Guidance literature:
-
Multi-step reaction with 10 steps
1.1: 47 percent HBr; AcOH / Heating
2.1: H2 / 10 percent Pd-C / ethyl acetate / atmospheric pressure
2.2: 8.0 g / p-TsOH*H2O / Heating
3.1: aq. NaOH / ethanol / 1 h
4.1: SOCl2; DMF / toluene
5.1: 4.5 g / AlCl3 / 1,2-dichloro-ethane / 1 h / 20 °C
6.1: 82 percent / NH2OH*HCl; AcONa / H2O; ethanol / 2 h / Heating
7.1: 63 percent / polyphosphoric acid / 0.33 h / 120 °C
8.1: 89 percent / NaH / dimethylformamide / 4 h / 20 °C
9.1: 80 percent / N-chlorosuccinimide / dimethylformamide / 7 h / 70 °C
10.1: LDA / hexane; tetrahydrofuran / 0.25 h / 0 °C
10.2: 16 percent / hexane; tetrahydrofuran / 1.25 h / -78 - 0 °C
With
sodium hydroxide; N-chloro-succinimide; aluminium trichloride; thionyl chloride; PPA; hydroxylamine hydrochloride; hydrogen bromide; hydrogen; sodium acetate; sodium hydride; acetic acid; N,N-dimethyl-formamide; lithium diisopropyl amide;
palladium on activated charcoal;
In
tetrahydrofuran; ethanol; hexane; water; ethyl acetate; 1,2-dichloro-ethane; N,N-dimethyl-formamide; toluene;
5.1: intramolecular Friedel-Crafts acylation / 7.1: Beckmann rearrangement;
DOI:10.1016/S0968-0896(01)00289-9
