Technology Process of 9-(4,6-dimethylpyrimidin-2-yl)-4-((1-methyl-4-phenyl-1H-pyrazol-3-yl)methyl)-1,4,9-triazaspiro[5.5]undecan-5-one
There total 11 articles about 9-(4,6-dimethylpyrimidin-2-yl)-4-((1-methyl-4-phenyl-1H-pyrazol-3-yl)methyl)-1,4,9-triazaspiro[5.5]undecan-5-one which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
C30H39N7O3;
With
trifluoroacetic acid;
In
dichloromethane;
at 20 ℃;
for 1.5h;
With
sodium hydrogencarbonate;
In
dichloromethane; water;
pH=10;
- Guidance literature:
-
Multi-step reaction with 7 steps
1.1: sodium acetate; acetic acid; sodium tris(acetoxy)borohydride / dichloromethane / 0.67 h / Inert atmosphere
1.2: 0.08 h / 0 °C
2.1: trifluoroacetic acid / dichloromethane / 1.5 h / 20 °C / Inert atmosphere
2.2: 22 h / 0 °C / Reflux
3.1: N-ethyl-N,N-diisopropylamine / 1,2-dichloro-ethane / 112 h / 20 °C
4.1: hydrogen / 10 wt% Pd(OH)2 on carbon / tetrahydrofuran; methanol / 20 °C / 37503.8 Torr
5.1: N-ethyl-N,N-diisopropylamine / ethanol / 1 h / 120 °C / microwave irradiation; sealed tube
6.1: sodium hydride / tetra-(n-butyl)ammonium iodide / tetrahydrofuran / 0.67 h / 0 °C
6.2: 5.5 h / 0 - 20 °C
7.1: potassium phosphate / palladium diacetate; dicyclohexyl-(2',6'-dimethoxybiphenyl-2-yl)-phosphane / toluene / 16 h / 93 °C / Inert atmosphere
7.2: 1.5 h / 20 °C
7.3: pH 10
With
potassium phosphate; hydrogen; sodium acetate; sodium tris(acetoxy)borohydride; sodium hydride; acetic acid; N-ethyl-N,N-diisopropylamine; trifluoroacetic acid;
dicyclohexyl-(2',6'-dimethoxybiphenyl-2-yl)-phosphane; 10 wt% Pd(OH)2 on carbon; palladium diacetate; tetra-(n-butyl)ammonium iodide;
In
tetrahydrofuran; methanol; ethanol; dichloromethane; 1,2-dichloro-ethane; toluene;
- Guidance literature:
-
Multi-step reaction with 3 steps
1.1: N-ethyl-N,N-diisopropylamine / ethanol / 1 h / 120 °C / microwave irradiation; sealed tube
2.1: sodium hydride / tetra-(n-butyl)ammonium iodide / tetrahydrofuran / 0.67 h / 0 °C
2.2: 5.5 h / 0 - 20 °C
3.1: potassium phosphate / palladium diacetate; dicyclohexyl-(2',6'-dimethoxybiphenyl-2-yl)-phosphane / toluene / 16 h / 93 °C / Inert atmosphere
3.2: 1.5 h / 20 °C
3.3: pH 10
With
potassium phosphate; sodium hydride; N-ethyl-N,N-diisopropylamine;
dicyclohexyl-(2',6'-dimethoxybiphenyl-2-yl)-phosphane; palladium diacetate; tetra-(n-butyl)ammonium iodide;
In
tetrahydrofuran; ethanol; toluene;