Technology Process of 10,10-dimethyl-7-thiatricyclo[6.3.0.0[2,6]]undeca-1(8),2(6)-dien-5-one
There total 10 articles about 10,10-dimethyl-7-thiatricyclo[6.3.0.0[2,6]]undeca-1(8),2(6)-dien-5-one which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
With
sulfuric acid;
at 90 ℃;
- Guidance literature:
-
Multi-step reaction with 7 steps
1.1: trichlorophosphate / dichloromethane / 1.5 h / 0 - 20 °C / Inert atmosphere
1.2: 19 h / Reflux
1.3: 0.75 h / Cooling with ice
2.1: triethylamine / dichloromethane / 6 h / Inert atmosphere; Reflux
3.1: water; lithium hydroxide / ethanol; tetrahydrofuran / 4 h / 60 °C
3.2: 20 °C / pH 1.5
4.1: thionyl chloride / N,N-dimethyl-formamide / toluene / 1 h / Reflux
5.1: N-ethyl-N,N-diisopropylamine / dichloromethane / 18 h / 0 - 20 °C / Inert atmosphere
6.1: tetrahydrofuran / 2.5 h / -70 - 0 °C / Inert atmosphere
6.2: -70 - -10 °C
7.1: sulfuric acid / 90 °C
With
thionyl chloride; sulfuric acid; water; triethylamine; N-ethyl-N,N-diisopropylamine; lithium hydroxide; trichlorophosphate;
N,N-dimethyl-formamide;
In
tetrahydrofuran; ethanol; dichloromethane; toluene;
- Guidance literature:
-
Multi-step reaction with 8 steps
1.1: copper(l) iodide / diethyl ether / 3.5 h / 0 °C / Inert atmosphere
1.2: 3.5 h / 0 °C
1.3: 0.5 h
2.1: trichlorophosphate / dichloromethane / 1.5 h / 0 - 20 °C / Inert atmosphere
2.2: 19 h / Reflux
2.3: 0.75 h / Cooling with ice
3.1: triethylamine / dichloromethane / 6 h / Inert atmosphere; Reflux
4.1: water; lithium hydroxide / ethanol; tetrahydrofuran / 4 h / 60 °C
4.2: 20 °C / pH 1.5
5.1: thionyl chloride / N,N-dimethyl-formamide / toluene / 1 h / Reflux
6.1: N-ethyl-N,N-diisopropylamine / dichloromethane / 18 h / 0 - 20 °C / Inert atmosphere
7.1: tetrahydrofuran / 2.5 h / -70 - 0 °C / Inert atmosphere
7.2: -70 - -10 °C
8.1: sulfuric acid / 90 °C
With
copper(l) iodide; thionyl chloride; sulfuric acid; water; triethylamine; N-ethyl-N,N-diisopropylamine; lithium hydroxide; trichlorophosphate;
N,N-dimethyl-formamide;
In
tetrahydrofuran; diethyl ether; ethanol; dichloromethane; toluene;