Technology Process of (-)-(cis)-7-bromo-8,12-difluoro-1,3,4,14b-tetrahydro-2H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepine-1-amine (4S)-2-hydroxy-5,5-dimethyl-4-phenyl-1,3,2-dioxaphosphorinane 2-oxide (1 : 1)
There total 9 articles about (-)-(cis)-7-bromo-8,12-difluoro-1,3,4,14b-tetrahydro-2H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepine-1-amine (4S)-2-hydroxy-5,5-dimethyl-4-phenyl-1,3,2-dioxaphosphorinane 2-oxide (1 : 1) which
guide to synthetic route it.
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synthetic route:
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1016235-10-1
(-)-(cis)-7-bromo-8,12-difluoro-1,3,4,14b-tetrahydro-2H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepine-1-amine (4S)-2-hydroxy-5,5-dimethyl-4-phenyl-1,3,2-dioxaphosphorinane 2-oxide (1 : 1)
- Guidance literature:
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In
ethanol; dichloromethane; isopropyl alcohol;
at 40 ℃;
Resolution of racemate;
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1016235-10-1
(-)-(cis)-7-bromo-8,12-difluoro-1,3,4,14b-tetrahydro-2H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepine-1-amine (4S)-2-hydroxy-5,5-dimethyl-4-phenyl-1,3,2-dioxaphosphorinane 2-oxide (1 : 1)
- Guidance literature:
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Multi-step reaction with 9 steps
1.1: sulfuric acid; nitric acid / dichloromethane; water / 1 h / 0 °C
2.1: sodium dithionite; water / ethanol / 1 h / Heating / reflux
3.1: toluene-4-sulfonic acid / toluene / 0.5 h / Heating / reflux; Dean-Stark apparatus
4.1: caesium carbonate / N,N-dimethyl-formamide / 3 h / 50 °C
5.1: xylene / 72 h / 150 °C
6.1: diphenyl phosphoryl azide; triethylamine / toluene / 2 h / Heating / reflux
6.2: 70 °C
7.1: borane-THF / tetrahydrofuran / 2 h / 30 °C
8.1: hydrogen bromide / acetic acid / 100 °C
8.2: pH 9
9.1: ethanol; dichloromethane; isopropyl alcohol / 40 °C / Resolution of racemate
With
sodium dithionite; borane-THF; sulfuric acid; diphenyl phosphoryl azide; water; hydrogen bromide; nitric acid; caesium carbonate; triethylamine;
toluene-4-sulfonic acid;
In
tetrahydrofuran; ethanol; dichloromethane; water; acetic acid; N,N-dimethyl-formamide; isopropyl alcohol; toluene; xylene;
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1016235-10-1
(-)-(cis)-7-bromo-8,12-difluoro-1,3,4,14b-tetrahydro-2H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepine-1-amine (4S)-2-hydroxy-5,5-dimethyl-4-phenyl-1,3,2-dioxaphosphorinane 2-oxide (1 : 1)
- Guidance literature:
-
Multi-step reaction with 7 steps
1.1: toluene-4-sulfonic acid / toluene / 0.5 h / Heating / reflux; Dean-Stark apparatus
2.1: caesium carbonate / N,N-dimethyl-formamide / 3 h / 50 °C
3.1: xylene / 72 h / 150 °C
4.1: diphenyl phosphoryl azide; triethylamine / toluene / 2 h / Heating / reflux
4.2: 70 °C
5.1: borane-THF / tetrahydrofuran / 2 h / 30 °C
6.1: hydrogen bromide / acetic acid / 100 °C
6.2: pH 9
7.1: ethanol; dichloromethane; isopropyl alcohol / 40 °C / Resolution of racemate
With
borane-THF; diphenyl phosphoryl azide; hydrogen bromide; caesium carbonate; triethylamine;
toluene-4-sulfonic acid;
In
tetrahydrofuran; ethanol; dichloromethane; acetic acid; N,N-dimethyl-formamide; isopropyl alcohol; toluene; xylene;