Technology Process of [2,3-dihydro-2,3-dimethoxy-2,3-dimethylbenzo[b][1,4]dioxin-7-yl]diphenylphosphine
There total 8 articles about [2,3-dihydro-2,3-dimethoxy-2,3-dimethylbenzo[b][1,4]dioxin-7-yl]diphenylphosphine which
guide to synthetic route it.
The literature collected by LookChem mainly comes from the sharing of users and the free literature resources found by Internet computing technology. We keep the original model of the professional version of literature to make it easier and faster for users to retrieve and use. At the same time, we analyze and calculate the most feasible synthesis route with the highest yield for your reference as below:
synthetic route:
- Guidance literature:
-
(2R,3R)-6-bromo-2,3-dihydro-2,3-dimethoxy-2,3-dimethylbenzo[b][1,4]dioxin;
With
n-butyllithium;
In
tetrahydrofuran; hexane;
at -75 ℃;
for 2h;
Inert atmosphere;
chloro-diphenylphosphine;
In
tetrahydrofuran; hexane;
at -75 - 0 ℃;
for 3.75h;
Inert atmosphere;
DOI:10.1016/j.tetlet.2011.11.111
- Guidance literature:
-
Multi-step reaction with 7 steps
1.1: nitric acid; acetic acid / 17 h / 15 - 20 °C / Inert atmosphere
2.1: 20% palladium hydroxide on charcoal; hydrogen / methanol / 2 h / 3102.97 Torr
3.1: N,N-dimethyl-formamide / 2.5 h / 20 °C / Inert atmosphere
3.2: 2 h / 20 °C / Inert atmosphere; Cooling with ice
4.1: isopropyl alcohol / 12 h / 20 °C / Inert atmosphere
5.1: sodium hydroxide / 18 h / 100 °C / Inert atmosphere
6.1: acetic acid; sodium nitrite / water; acetonitrile / 0.5 h / 0 - 5 °C / Inert atmosphere
6.2: 1 h / 55 - 60 °C / Inert atmosphere
7.1: n-butyllithium / tetrahydrofuran; hexane / 2 h / -75 °C / Inert atmosphere
7.2: 3.75 h / -75 - 0 °C / Inert atmosphere
With
n-butyllithium; 20% palladium hydroxide on charcoal; hydrogen; nitric acid; acetic acid; sodium hydroxide; sodium nitrite;
In
tetrahydrofuran; methanol; hexane; water; N,N-dimethyl-formamide; isopropyl alcohol; acetonitrile;
DOI:10.1016/j.tetlet.2011.11.111
- Guidance literature:
-
Multi-step reaction with 6 steps
1.1: 20% palladium hydroxide on charcoal; hydrogen / methanol / 2 h / 3102.97 Torr
2.1: N,N-dimethyl-formamide / 2.5 h / 20 °C / Inert atmosphere
2.2: 2 h / 20 °C / Inert atmosphere; Cooling with ice
3.1: isopropyl alcohol / 12 h / 20 °C / Inert atmosphere
4.1: sodium hydroxide / 18 h / 100 °C / Inert atmosphere
5.1: acetic acid; sodium nitrite / water; acetonitrile / 0.5 h / 0 - 5 °C / Inert atmosphere
5.2: 1 h / 55 - 60 °C / Inert atmosphere
6.1: n-butyllithium / tetrahydrofuran; hexane / 2 h / -75 °C / Inert atmosphere
6.2: 3.75 h / -75 - 0 °C / Inert atmosphere
With
n-butyllithium; 20% palladium hydroxide on charcoal; hydrogen; acetic acid; sodium hydroxide; sodium nitrite;
In
tetrahydrofuran; methanol; hexane; water; N,N-dimethyl-formamide; isopropyl alcohol; acetonitrile;
DOI:10.1016/j.tetlet.2011.11.111
![(2R,3R)-6-bromo-2,3-dihydro-2,3-dimethoxy-2,3-dimethylbenzo[b][1,4]dioxin](/Databaselist/images/loading.webp)
