Technology Process of (3aα,4aS*,15bβ,15cα)-(+/-)-10-oxo-3a,6,7,15b,15c-pentahydro-2,2-dimethyl-5H-<1,3>dioxolo<4,5-h>-1,3-dioxolo<4,5>cyclopenta<1,2-a>pyrrolo-<2,1-b><3>benzazepin-9(4H)-one
There total 1 articles about (3aα,4aS*,15bβ,15cα)-(+/-)-10-oxo-3a,6,7,15b,15c-pentahydro-2,2-dimethyl-5H-<1,3>dioxolo<4,5-h>-1,3-dioxolo<4,5>cyclopenta<1,2-a>pyrrolo-<2,1-b><3>benzazepin-9(4H)-one which
guide to synthetic route it.
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synthetic route:
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130552-96-4,130609-67-5
(3aα,4aS*,10β,15bβ,15cα)-(+/-)-10-phenylthio-3a,6,7,10,15b,15c-hexahydro-2,2-dimethyl-5H-<1,3>dioxolo<4,5-h>-1,3-dioxolo<4,5>cyclopenta<1,2-a>pyrrolo<2,1-b><3>benzazepin-9(4H)-one
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130552-98-6
(3aα,4aS*,15bβ,15cα)-(+/-)-10-oxo-3a,6,7,15b,15c-pentahydro-2,2-dimethyl-5H-<1,3>dioxolo<4,5-h>-1,3-dioxolo<4,5>cyclopenta<1,2-a>pyrrolo-<2,1-b><3>benzazepin-9(4H)-one
- Guidance literature:
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With
potassium hydride;
In
tetrahydrofuran;
for 3h;
Yield given;
Ambient temperature;
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130552-98-6
(3aα,4aS*,15bβ,15cα)-(+/-)-10-oxo-3a,6,7,15b,15c-pentahydro-2,2-dimethyl-5H-<1,3>dioxolo<4,5-h>-1,3-dioxolo<4,5>cyclopenta<1,2-a>pyrrolo-<2,1-b><3>benzazepin-9(4H)-one
- Guidance literature:
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Multi-step reaction with 6 steps
1: 81 percent / BH3*THF / tetrahydrofuran / 1.) -78 deg C, 12 h, 2.) -78 deg C to RT, 15 h
2: 96 percent / pyridine, DMAP / CH2Cl2 / 3 h / Ambient temperature
3: 90 percent / 1 N aq. HCl / tetrahydrofuran / 6.5 h / Ambient temperature
4: 89 percent / 1.) DMSO, trifluoroacetic anhydride, 2.) Et3N / 1.) CH2Cl2, -78 deg C, 1.5 h, 2.) 0 deg C, 0.5 h
5: 43 percent / p-toluenesulfonic acid monohydrate / diethyl ether / 6 h / Heating
6: 88 percent / NaBH4 / methanol; CH2Cl2 / 3 h / Ambient temperature
With
pyridine; hydrogenchloride; dmap; sodium tetrahydroborate; borane-THF; toluene-4-sulfonic acid; dimethyl sulfoxide; triethylamine; trifluoroacetic anhydride;
In
tetrahydrofuran; methanol; diethyl ether; dichloromethane;
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130552-98-6
(3aα,4aS*,15bβ,15cα)-(+/-)-10-oxo-3a,6,7,15b,15c-pentahydro-2,2-dimethyl-5H-<1,3>dioxolo<4,5-h>-1,3-dioxolo<4,5>cyclopenta<1,2-a>pyrrolo-<2,1-b><3>benzazepin-9(4H)-one
- Guidance literature:
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Multi-step reaction with 7 steps
1: 81 percent / BH3*THF / tetrahydrofuran / 1.) -78 deg C, 12 h, 2.) -78 deg C to RT, 15 h
2: 96 percent / pyridine, DMAP / CH2Cl2 / 3 h / Ambient temperature
3: 90 percent / 1 N aq. HCl / tetrahydrofuran / 6.5 h / Ambient temperature
4: 89 percent / 1.) DMSO, trifluoroacetic anhydride, 2.) Et3N / 1.) CH2Cl2, -78 deg C, 1.5 h, 2.) 0 deg C, 0.5 h
5: 43 percent / p-toluenesulfonic acid monohydrate / diethyl ether / 6 h / Heating
6: 88 percent / NaBH4 / methanol; CH2Cl2 / 3 h / Ambient temperature
7: 83 percent / 1N HCl / tetrahydrofuran / 5 h / Ambient temperature
With
pyridine; hydrogenchloride; dmap; sodium tetrahydroborate; borane-THF; toluene-4-sulfonic acid; dimethyl sulfoxide; triethylamine; trifluoroacetic anhydride;
In
tetrahydrofuran; methanol; diethyl ether; dichloromethane;
