Technology Process of S-2-(2,4-difluorophenylamino)-8-(2,2-dimethyl-[1,3]dioxolan-4-ylmethoxy)-10,11-dihydro-dibenzo[a,d]cyclohepten-5-one
There total 9 articles about S-2-(2,4-difluorophenylamino)-8-(2,2-dimethyl-[1,3]dioxolan-4-ylmethoxy)-10,11-dihydro-dibenzo[a,d]cyclohepten-5-one which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
With
palladium diacetate; sodium t-butanolate; XPhos;
In
toluene; tert-butyl alcohol;
at 90 ℃;
for 2h;
Inert atmosphere;
DOI:10.1021/jm300327h
- Guidance literature:
-
Multi-step reaction with 6 steps
1.1: triphenylphosphine / methanol / Reflux
1.2: Reflux
2.1: hydrogen / palladium 10% on activated carbon / ethyl acetate; acetonitrile; methanol / 4 h
3.1: thionyl chloride / dichloromethane / 2 h / Reflux
3.2: 1.25 h / 20 °C
3.3: Cooling with ice
4.1: hydrogen bromide; acetic acid / water / 3 h / 120 - 130 °C
4.2: Cooling with ice
5.1: potassium carbonate / N,N-dimethyl-formamide / 24 h / 80 °C / Inert atmosphere
6.1: sodium t-butanolate; XPhos / palladium diacetate / toluene; tert-butyl alcohol / 3 h / 100 °C
With
thionyl chloride; hydrogen bromide; hydrogen; potassium carbonate; acetic acid; triphenylphosphine; sodium t-butanolate; XPhos;
palladium 10% on activated carbon; palladium diacetate;
In
methanol; dichloromethane; water; ethyl acetate; N,N-dimethyl-formamide; toluene; acetonitrile; tert-butyl alcohol;
- Guidance literature:
-
Multi-step reaction with 4 steps
1.1: thionyl chloride / dichloromethane / 2 h / Reflux
1.2: 1.25 h / 20 °C
1.3: Cooling with ice
2.1: hydrogen bromide; acetic acid / water / 3 h / 120 - 130 °C
2.2: Cooling with ice
3.1: potassium carbonate / N,N-dimethyl-formamide / 24 h / 80 °C / Inert atmosphere
4.1: sodium t-butanolate; XPhos / palladium diacetate / toluene; tert-butyl alcohol / 3 h / 100 °C
With
thionyl chloride; hydrogen bromide; potassium carbonate; acetic acid; sodium t-butanolate; XPhos;
palladium diacetate;
In
dichloromethane; water; N,N-dimethyl-formamide; toluene; tert-butyl alcohol;