Technology Process of 2-chloro-8-(3,3-difluoro-cyclobutyl)-6-methyl-5,6,7,8-tetrahydro-9-oxa-1,6-diaza-benzocycloheptene
There total 2 articles about 2-chloro-8-(3,3-difluoro-cyclobutyl)-6-methyl-5,6,7,8-tetrahydro-9-oxa-1,6-diaza-benzocycloheptene which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
Multi-step reaction with 10 steps
1.1: diethylamino-sulfur trifluoride / dichloromethane / 24 h / -10 - 20 °C
2.1: sodium hydroxide; water / pentane; methanol / 75 h / 20 - 60 °C
2.2: pH 1
3.1: caesium carbonate / N,N-dimethyl-formamide / 20 °C / Inert atmosphere
4.1: lithium aluminium tetrahydride / tetrahydrofuran / -30 - 20 °C / Inert atmosphere
4.2: 0 °C
5.1: pyridinium chlorochromate / dichloromethane / 1 h / 20 °C
6.1: N-ethyl-N,N-diisopropylamine / dichloromethane / 73 h / 0 - 20 °C
7.1: hydrogen / palladium 10% on activated carbon / methanol / 24 h / 20 °C / 2327.23 Torr
8.1: caesium carbonate / N,N-dimethyl-formamide / 20 °C
9.1: sodium hydride / tetrahydrofuran / 0 - 40 °C
10.1: methanol / 6 h / 20 °C
10.2: 20 °C
With
lithium aluminium tetrahydride; diethylamino-sulfur trifluoride; water; hydrogen; sodium hydride; caesium carbonate; N-ethyl-N,N-diisopropylamine; pyridinium chlorochromate; sodium hydroxide;
palladium 10% on activated carbon;
In
tetrahydrofuran; methanol; dichloromethane; N,N-dimethyl-formamide; pentane;
- Guidance literature:
-
Multi-step reaction with 11 steps
1.1: sodium periodate / ruthenium(III) trichloride hydrate / dichloromethane; acetonitrile; water / 5 - 20 °C
2.1: diethylamino-sulfur trifluoride / dichloromethane / 24 h / -10 - 20 °C
3.1: sodium hydroxide; water / pentane; methanol / 75 h / 20 - 60 °C
3.2: pH 1
4.1: caesium carbonate / N,N-dimethyl-formamide / 20 °C / Inert atmosphere
5.1: lithium aluminium tetrahydride / tetrahydrofuran / -30 - 20 °C / Inert atmosphere
5.2: 0 °C
6.1: pyridinium chlorochromate / dichloromethane / 1 h / 20 °C
7.1: N-ethyl-N,N-diisopropylamine / dichloromethane / 73 h / 0 - 20 °C
8.1: hydrogen / palladium 10% on activated carbon / methanol / 24 h / 20 °C / 2327.23 Torr
9.1: caesium carbonate / N,N-dimethyl-formamide / 20 °C
10.1: sodium hydride / tetrahydrofuran / 0 - 40 °C
11.1: methanol / 6 h / 20 °C
11.2: 20 °C
With
sodium periodate; lithium aluminium tetrahydride; diethylamino-sulfur trifluoride; water; hydrogen; sodium hydride; caesium carbonate; N-ethyl-N,N-diisopropylamine; pyridinium chlorochromate; sodium hydroxide;
ruthenium(III) trichloride hydrate; palladium 10% on activated carbon;
In
tetrahydrofuran; methanol; dichloromethane; water; N,N-dimethyl-formamide; acetonitrile; pentane;