Technology Process of 3-({[3,3-dibutyl-7-(methyloxy)-1,1-dioxido-5-phenyl-2,3,4,5-tetrahydro-1,4-benzothiazepin-8-yl]methyl}amino)pentanedioic acid trifluoroacetate
There total 20 articles about 3-({[3,3-dibutyl-7-(methyloxy)-1,1-dioxido-5-phenyl-2,3,4,5-tetrahydro-1,4-benzothiazepin-8-yl]methyl}amino)pentanedioic acid trifluoroacetate which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
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;
With
water; lithium hydroxide;
In
tetrahydrofuran;
at 25 ℃;
for 4h;
trifluoroacetic acid;
In
water; acetonitrile;
- Guidance literature:
-
Multi-step reaction with 9 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
9.1: water; lithium hydroxide / tetrahydrofuran / 4 h / 25 °C
With
lithium aluminium tetrahydride; borane-THF; 1,3-bis-(diphenylphosphino)propane; water; dihydrogen peroxide; Dess-Martin periodane; acetic acid; triethylamine; trifluoroacetic acid; citric acid; potassium hydroxide; lithium hydroxide;
palladium diacetate;
In
tetrahydrofuran; ethanol; dichloromethane; water; dimethyl sulfoxide; 1,2-dichloro-ethane; toluene;
- Guidance literature:
-
Multi-step reaction with 11 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
11.1: water; lithium hydroxide / tetrahydrofuran / 4 h / 25 °C
With
chlorosulfonic acid; lithium aluminium tetrahydride; borane-THF; 1,3-bis-(diphenylphosphino)propane; water; dihydrogen peroxide; Dess-Martin periodane; acetic acid; triethylamine; trifluoroacetic acid; citric acid; potassium hydroxide; lithium hydroxide;
palladium diacetate;
In
tetrahydrofuran; ethanol; dichloromethane; water; dimethyl sulfoxide; ethyl acetate; 1,2-dichloro-ethane; toluene;