Technology Process of N-methyl-N-phenyl-5-oxa-1-azaspiro[2.5]oct-1-en-2-amine
There total 9 articles about N-methyl-N-phenyl-5-oxa-1-azaspiro[2.5]oct-1-en-2-amine which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
N-methyl-N-phenyltetrahydropyran-3-thiocarboxamide;
With
phosgene;
In
dichloromethane; N,N-dimethyl-formamide; toluene;
at 0 - 20 ℃;
With
1,4-diaza-bicyclo[2.2.2]octane;
In
tetrahydrofuran;
at 20 ℃;
for 0.666667h;
With
sodium azide;
at 20 ℃;
for 4h;
Inert atmosphere;
DOI:10.3987/COM-10-S(E)73
- Guidance literature:
-
Multi-step reaction with 7 steps
1.1: pyridinium chlorochromate / dichloromethane / 2.5 h / 20 °C / Molecular sieve
2.1: potassium tert-butylate / 1,2-dimethoxyethane; tert-butyl alcohol / 3.5 h / 0 - 20 °C
3.1: sodium hydroxide / ethanol; water / 2.5 h / Reflux
4.1: thionyl chloride / 2 h / Reflux
5.1: triethylamine / dichloromethane / 4 h / 20 °C
6.1: Lawessons reagent / toluene / 2.5 h / 110 °C
7.1: phosgene / dichloromethane; N,N-dimethyl-formamide; toluene / 0 - 20 °C
7.2: 0.67 h / 20 °C
7.3: 4 h / 20 °C / Inert atmosphere
With
Lawessons reagent; phosgene; thionyl chloride; potassium tert-butylate; triethylamine; pyridinium chlorochromate; sodium hydroxide;
In
1,2-dimethoxyethane; ethanol; dichloromethane; water; N,N-dimethyl-formamide; toluene; tert-butyl alcohol;
DOI:10.3987/COM-10-S(E)73
- Guidance literature:
-
Multi-step reaction with 9 steps
1.1: borane-THF / tetrahydrofuran / 3 h / 0 °C
2.1: dihydrogen peroxide; sodium hydroxide / tetrahydrofuran; water / 0 - 20 °C
3.1: pyridinium chlorochromate / dichloromethane / 2.5 h / 20 °C / Molecular sieve
4.1: potassium tert-butylate / 1,2-dimethoxyethane; tert-butyl alcohol / 3.5 h / 0 - 20 °C
5.1: sodium hydroxide / ethanol; water / 2.5 h / Reflux
6.1: thionyl chloride / 2 h / Reflux
7.1: triethylamine / dichloromethane / 4 h / 20 °C
8.1: Lawessons reagent / toluene / 2.5 h / 110 °C
9.1: phosgene / dichloromethane; N,N-dimethyl-formamide; toluene / 0 - 20 °C
9.2: 0.67 h / 20 °C
9.3: 4 h / 20 °C / Inert atmosphere
With
Lawessons reagent; phosgene; thionyl chloride; borane-THF; potassium tert-butylate; dihydrogen peroxide; triethylamine; pyridinium chlorochromate; sodium hydroxide;
In
tetrahydrofuran; 1,2-dimethoxyethane; ethanol; dichloromethane; water; N,N-dimethyl-formamide; toluene; tert-butyl alcohol;
DOI:10.3987/COM-10-S(E)73
