Technology Process of cyclobutyl[9-(4-fluorobenzyl)-7,7a,8,9,10,11-hexahydropyrazino[1,2-d]pyrido[3,2-b][1,4]diazepin-5(6H)-yl]methanone
There total 8 articles about cyclobutyl[9-(4-fluorobenzyl)-7,7a,8,9,10,11-hexahydropyrazino[1,2-d]pyrido[3,2-b][1,4]diazepin-5(6H)-yl]methanone which
guide to synthetic route it.
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synthetic route:
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1350460-11-5
9-(4-fluorobenzyl)-5,6,7,7a,8,9,10,11-octahydropyrazino[1,2-d]pyrido[3,2-b][1,4]diazepine
- Guidance literature:
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9-(4-fluorobenzyl)-5,6,7,7a,8,9,10,11-octahydropyrazino[1,2-d]pyrido[3,2-b][1,4]diazepine; Cyclobutanecarbonyl chloride;
In
dichloromethane;
at 20 ℃;
for 12h;
With
sodium carbonate;
In
dichloromethane;
for 0.5h;
With
sodium hydroxide;
In
dichloromethane;
pH=~ 9;
- Guidance literature:
-
Multi-step reaction with 8 steps
1.1: hydrogenchloride; hydrogen / 20% palladium hydroxide-activated charcoal / water; methanol / 22 h / 20 °C / 1551.49 Torr
2.1: potassium carbonate / ethyl acetate; water / 22 h / 20 °C / 1551.49 Torr
2.2: 3.08 h / 20 °C / Cooling with ice
3.1: N-ethyl-N,N-diisopropylamine / dimethyl sulfoxide / 7 h / 95 °C / Inert atmosphere
4.1: hydrogen / platinum(IV) oxide / methanol / 54 h / 760.05 Torr
4.2: 41 h / Reflux
5.1: dichloromethane / 1.85 h / 0 - 20 °C
6.1: sodium hydroxide / dichloromethane
6.2: 13 h / 20 °C
7.1: lithium aluminium tetrahydride / tetrahydrofuran / 1 h / Reflux; Inert atmosphere
7.2: Inert atmosphere; Cooling with ice
8.1: dichloromethane / 12 h / 20 °C
8.2: 0.5 h
8.3: pH ~ 9
With
hydrogenchloride; lithium aluminium tetrahydride; hydrogen; potassium carbonate; N-ethyl-N,N-diisopropylamine; sodium hydroxide;
platinum(IV) oxide; 20% palladium hydroxide-activated charcoal;
In
tetrahydrofuran; methanol; dichloromethane; water; dimethyl sulfoxide; ethyl acetate;
- Guidance literature:
-
Multi-step reaction with 6 steps
1.1: N-ethyl-N,N-diisopropylamine / dimethyl sulfoxide / 7 h / 95 °C / Inert atmosphere
2.1: hydrogen / platinum(IV) oxide / methanol / 54 h / 760.05 Torr
2.2: 41 h / Reflux
3.1: dichloromethane / 1.85 h / 0 - 20 °C
4.1: sodium hydroxide / dichloromethane
4.2: 13 h / 20 °C
5.1: lithium aluminium tetrahydride / tetrahydrofuran / 1 h / Reflux; Inert atmosphere
5.2: Inert atmosphere; Cooling with ice
6.1: dichloromethane / 12 h / 20 °C
6.2: 0.5 h
6.3: pH ~ 9
With
lithium aluminium tetrahydride; hydrogen; N-ethyl-N,N-diisopropylamine; sodium hydroxide;
platinum(IV) oxide;
In
tetrahydrofuran; methanol; dichloromethane; dimethyl sulfoxide;