Technology Process of dimethyl 3-({[3,3-dibutyl-7-(methyloxy)-1,1-dioxido-5-phenyl-2,3,4,5-tetrahydro-1,4-benzothiazepin-8-yl]methyl}amino)pentanedioate
There total 20 articles about dimethyl 3-({[3,3-dibutyl-7-(methyloxy)-1,1-dioxido-5-phenyl-2,3,4,5-tetrahydro-1,4-benzothiazepin-8-yl]methyl}amino)pentanedioate 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:
-
3,3-dibutyl-7-(methyloxy)-5-phenyl-2,3,4,5-tetrahydro-1,4-benzothiazepine-8-carbaldehyde 1,1-dioxide; 3-aminoglutaric acid dimethyl ester;
With
acetic acid;
In
1,2-dichloro-ethane;
at 25 ℃;
for 1h;
With
sodium tris(acetoxy)borohydride;
In
1,2-dichloro-ethane;
for 19h;
With
sodium carbonate;
In
dichloromethane; water; 1,2-dichloro-ethane;
- Guidance literature:
-
Multi-step reaction with 8 steps
1.1: potassium hydroxide / ethanol; water / 18 h / 70 °C / Reflux
1.2: 15 h / 85 °C
2.1: citric acid / toluene / 50 h / 130 °C / Reflux
3.1: triethylamine; 1,3-bis-(diphenylphosphino)propane / palladium diacetate / dimethyl sulfoxide / 42 h / 70 °C
4.1: lithium aluminium tetrahydride / tetrahydrofuran / 0.25 h / 25 °C
4.2: 0.5 h
5.1: borane-THF / tetrahydrofuran / 2 h / 25 °C
6.1: trifluoroacetic acid; dihydrogen peroxide / water / 1 h / 25 °C
6.2: 1 h / pH 12 / Cooling with ice
7.1: Dess-Martin periodane / dichloromethane / 1 h / 25 °C
8.1: acetic acid / 1,2-dichloro-ethane / 1 h / 25 °C
8.2: 19 h
With
lithium aluminium tetrahydride; borane-THF; 1,3-bis-(diphenylphosphino)propane; dihydrogen peroxide; Dess-Martin periodane; acetic acid; triethylamine; trifluoroacetic acid; citric acid; potassium hydroxide;
palladium diacetate;
In
tetrahydrofuran; ethanol; dichloromethane; water; dimethyl sulfoxide; 1,2-dichloro-ethane; toluene;
- Guidance literature:
-
Multi-step reaction with 10 steps
1.1: lithium aluminium tetrahydride / tetrahydrofuran / 20 - 65 °C
1.2: 2 h / 0 °C
2.1: chlorosulfonic acid / ethyl acetate / 3 h / 25 - 40 °C
3.1: potassium hydroxide / ethanol; water / 18 h / 70 °C / Reflux
3.2: 15 h / 85 °C
4.1: citric acid / toluene / 50 h / 130 °C / Reflux
5.1: triethylamine; 1,3-bis-(diphenylphosphino)propane / palladium diacetate / dimethyl sulfoxide / 42 h / 70 °C
6.1: lithium aluminium tetrahydride / tetrahydrofuran / 0.25 h / 25 °C
6.2: 0.5 h
7.1: borane-THF / tetrahydrofuran / 2 h / 25 °C
8.1: trifluoroacetic acid; dihydrogen peroxide / water / 1 h / 25 °C
8.2: 1 h / pH 12 / Cooling with ice
9.1: Dess-Martin periodane / dichloromethane / 1 h / 25 °C
10.1: acetic acid / 1,2-dichloro-ethane / 1 h / 25 °C
10.2: 19 h
With
chlorosulfonic acid; lithium aluminium tetrahydride; borane-THF; 1,3-bis-(diphenylphosphino)propane; dihydrogen peroxide; Dess-Martin periodane; acetic acid; triethylamine; trifluoroacetic acid; citric acid; potassium hydroxide;
palladium diacetate;
In
tetrahydrofuran; ethanol; dichloromethane; water; dimethyl sulfoxide; ethyl acetate; 1,2-dichloro-ethane; toluene;
