Technology Process of 5-(5-(3-fluoro-4-hydroxyphenyl)-8-oxo-6-thioxo-5,7-diazaspiro[3.4]octan-7-yl)-3-(trifluoromethyl)picolinonitrile
There total 6 articles about 5-(5-(3-fluoro-4-hydroxyphenyl)-8-oxo-6-thioxo-5,7-diazaspiro[3.4]octan-7-yl)-3-(trifluoromethyl)picolinonitrile which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
5-amino-3-(trifluoromethyl)pyridine-2-carbonitrile; thiophosgene; 1-((3-fluoro-4-hydroxyphenyl)amino)cyclobutanecarbonitrile;
In
N,N-dimethyl acetamide;
at 60 ℃;
for 18h;
With
hydrogenchloride; water;
In
methanol; N,N-dimethyl acetamide;
for 2h;
Reflux;
- Guidance literature:
-
Multi-step reaction with 5 steps
1.1: trichlorophosphate / N,N-dimethyl-formamide / 4 h / 110 °C
2.1: sodium t-butanolate / tris-(dibenzylideneacetone)dipalladium(0); 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene / toluene / 2 h / Reflux; Inert atmosphere
3.1: 1,1'-bis-(diphenylphosphino)ferrocene; tris-(dibenzylideneacetone)dipalladium(0) / N,N-dimethyl-formamide / 0.5 h / 170 °C / Reflux; Inert atmosphere
4.1: trifluoroacetic acid / dichloromethane / 3 h / 20 °C
5.1: N,N-dimethyl acetamide / 18 h / 60 °C
5.2: 2 h / Reflux
With
trifluoroacetic acid; sodium t-butanolate; trichlorophosphate;
1,1'-bis-(diphenylphosphino)ferrocene; tris-(dibenzylideneacetone)dipalladium(0); 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene;
In
dichloromethane; N,N-dimethyl acetamide; N,N-dimethyl-formamide; toluene;
- Guidance literature:
-
Multi-step reaction with 4 steps
1.1: sodium t-butanolate / tris-(dibenzylideneacetone)dipalladium(0); 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene / toluene / 2 h / Reflux; Inert atmosphere
2.1: 1,1'-bis-(diphenylphosphino)ferrocene; tris-(dibenzylideneacetone)dipalladium(0) / N,N-dimethyl-formamide / 0.5 h / 170 °C / Reflux; Inert atmosphere
3.1: trifluoroacetic acid / dichloromethane / 3 h / 20 °C
4.1: N,N-dimethyl acetamide / 18 h / 60 °C
4.2: 2 h / Reflux
With
trifluoroacetic acid; sodium t-butanolate;
1,1'-bis-(diphenylphosphino)ferrocene; tris-(dibenzylideneacetone)dipalladium(0); 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene;
In
dichloromethane; N,N-dimethyl acetamide; N,N-dimethyl-formamide; toluene;
