Technology Process of (R)-6,6-difluoro-5-(2-fluoro-5-(tetrahydro-2H-pyran-4-yl)phenyl)-5,7,7-trimethyl-1,4-oxazepan-3-one
There total 11 articles about (R)-6,6-difluoro-5-(2-fluoro-5-(tetrahydro-2H-pyran-4-yl)phenyl)-5,7,7-trimethyl-1,4-oxazepan-3-one which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
With
hydrogen;
palladium 10% on activated carbon;
In
ethyl acetate;
at 20 ℃;
for 16h;
- Guidance literature:
-
Multi-step reaction with 9 steps
1: zinc / tetrahydrofuran / 5 h / Inert atmosphere; Reflux
2: tetrahydrofuran; 2-methyltetrahydrofuran / 18 h / -78 - 23 °C
3: tetrakis(triphenylphosphine) palladium(0) / tetrahydrofuran / 8 h / 23 - 70 °C / Inert atmosphere
4: sodium periodate / ruthenium trichloride / ethyl acetate; acetonitrile; water / 3 h / 23 °C
5: thionyl chloride / 18 h / 23 °C / Reflux
6: dichloromethane / 0.5 h / 0 - 23 °C
7: trimethylaluminum / toluene / 2 h / 23 °C
8: lithium tert-butoxide; XPhos / bis(dibenzylideneacetone)-palladium(0) / 1,4-dioxane / 16 h / 110 °C / Microwave
9: hydrogen / palladium 10% on activated carbon / ethyl acetate / 16 h / 20 °C
With
sodium periodate; thionyl chloride; hydrogen; trimethylaluminum; lithium tert-butoxide; zinc; XPhos;
ruthenium trichloride; tetrakis(triphenylphosphine) palladium(0); palladium 10% on activated carbon; bis(dibenzylideneacetone)-palladium(0);
In
tetrahydrofuran; 2-methyltetrahydrofuran; 1,4-dioxane; dichloromethane; water; ethyl acetate; toluene; acetonitrile;
1: Reformatsky Reaction;
- Guidance literature:
-
Multi-step reaction with 8 steps
1: tetrahydrofuran; 2-methyltetrahydrofuran / 18 h / -78 - 23 °C
2: tetrakis(triphenylphosphine) palladium(0) / tetrahydrofuran / 8 h / 23 - 70 °C / Inert atmosphere
3: sodium periodate / ruthenium trichloride / ethyl acetate; acetonitrile; water / 3 h / 23 °C
4: thionyl chloride / 18 h / 23 °C / Reflux
5: dichloromethane / 0.5 h / 0 - 23 °C
6: trimethylaluminum / toluene / 2 h / 23 °C
7: lithium tert-butoxide; XPhos / bis(dibenzylideneacetone)-palladium(0) / 1,4-dioxane / 16 h / 110 °C / Microwave
8: hydrogen / palladium 10% on activated carbon / ethyl acetate / 16 h / 20 °C
With
sodium periodate; thionyl chloride; hydrogen; trimethylaluminum; lithium tert-butoxide; XPhos;
ruthenium trichloride; tetrakis(triphenylphosphine) palladium(0); palladium 10% on activated carbon; bis(dibenzylideneacetone)-palladium(0);
In
tetrahydrofuran; 2-methyltetrahydrofuran; 1,4-dioxane; dichloromethane; water; ethyl acetate; toluene; acetonitrile;