Technology Process of (9-(3',4',5'-trimethoxyphenyl)-6,7-dihydro-5H-benzo[7]annulene-3,4-diyl)bis(oxy)bis(tert-butyldimethylsilane)
There total 7 articles about (9-(3',4',5'-trimethoxyphenyl)-6,7-dihydro-5H-benzo[7]annulene-3,4-diyl)bis(oxy)bis(tert-butyldimethylsilane) which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
Multi-step reaction with 7 steps
1.1: potassium tert-butylate / tetrahydrofuran / 0.25 h / 0 °C / Inert atmosphere
1.2: 0 - 20 °C
2.1: hydrogen / palladium 10% on activated carbon / methanol / 24 h
3.1: methanesulfonic acid; phosphorus pentoxide / 12 h / Inert atmosphere
4.1: trimethylammonium heptachlorodialuminate / dichloromethane / 1 h / 80 °C / Microwave irradiation; Inert atmosphere
5.1: N-ethyl-N,N-diisopropylamine / N,N-dimethyl-formamide / 3 h / Inert atmosphere
6.1: n-butyllithium / tetrahydrofuran; hexanes / 1 h / -78 °C / Inert atmosphere
6.2: -78 - 20 °C
6.3: 20 °C
7.1: acetic acid / 20 °C / Inert atmosphere
With
n-butyllithium; methanesulfonic acid; phosphorus pentoxide; trimethylammonium heptachlorodialuminate; potassium tert-butylate; hydrogen; acetic acid; N-ethyl-N,N-diisopropylamine;
palladium 10% on activated carbon;
In
tetrahydrofuran; methanol; hexanes; dichloromethane; N,N-dimethyl-formamide;
1.1: Wittig Reaction;
- Guidance literature:
-
Multi-step reaction with 6 steps
1.1: hydrogen / palladium 10% on activated carbon / methanol / 24 h
2.1: methanesulfonic acid; phosphorus pentoxide / 12 h / Inert atmosphere
3.1: trimethylammonium heptachlorodialuminate / dichloromethane / 1 h / 80 °C / Microwave irradiation; Inert atmosphere
4.1: N-ethyl-N,N-diisopropylamine / N,N-dimethyl-formamide / 3 h / Inert atmosphere
5.1: n-butyllithium / tetrahydrofuran; hexanes / 1 h / -78 °C / Inert atmosphere
5.2: -78 - 20 °C
5.3: 20 °C
6.1: acetic acid / 20 °C / Inert atmosphere
With
n-butyllithium; methanesulfonic acid; phosphorus pentoxide; trimethylammonium heptachlorodialuminate; hydrogen; acetic acid; N-ethyl-N,N-diisopropylamine;
palladium 10% on activated carbon;
In
tetrahydrofuran; methanol; hexanes; dichloromethane; N,N-dimethyl-formamide;