Technology Process of methyl 3α-acetoxy-5β-chol-9(11),16-dien-24-oate
There total 6 articles about methyl 3α-acetoxy-5β-chol-9(11),16-dien-24-oate which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
(Z)-3α-acetoxy-5β-pregna-9(11),17(20)-diene; acrylic acid methyl ester;
With
ethylaluminum dichloride;
In
dichloromethane; toluene;
at 0 - 35 ℃;
for 20h;
Inert atmosphere;
With
water;
In
dichloromethane; toluene;
Product distribution / selectivity;
Cooling;
- Guidance literature:
-
Multi-step reaction with 6 steps
1.1: hydrogen / palladium 10% on activated carbon / N,N-dimethyl-formamide / 3 h / 25 - 35 °C / 3102.97 Torr
2.1: sulfuric acid / dichloromethane / 2.15 h / 10 - 35 °C
3.1: lithium tri-t-butoxyaluminum hydride / tetrahydrofuran / 2 h / -45 - -40 °C / Inert atmosphere
4.1: potassium tert-butylate / tetrahydrofuran / 1.33 h / 25 - 35 °C / Inert atmosphere
4.2: 3 - 5 h / 25 - 35 °C / Inert atmosphere
4.3: Cooling
5.1: triethylamine / dmap / tert-butyl methyl ether / 2 h / 25 - 35 °C / Inert atmosphere
6.1: ethylaluminum dichloride / dichloromethane; toluene / 20 h / 0 - 35 °C / Inert atmosphere
6.2: Cooling
With
sulfuric acid; potassium tert-butylate; hydrogen; ethylaluminum dichloride; lithium tri-t-butoxyaluminum hydride; triethylamine;
dmap; palladium 10% on activated carbon;
In
tetrahydrofuran; dichloromethane; tert-butyl methyl ether; N,N-dimethyl-formamide; toluene;
- Guidance literature:
-
Multi-step reaction with 5 steps
1.1: sulfuric acid / dichloromethane / 2.15 h / 10 - 35 °C
2.1: lithium tri-t-butoxyaluminum hydride / tetrahydrofuran / 2 h / -45 - -40 °C / Inert atmosphere
3.1: potassium tert-butylate / tetrahydrofuran / 1.33 h / 25 - 35 °C / Inert atmosphere
3.2: 3 - 5 h / 25 - 35 °C / Inert atmosphere
3.3: Cooling
4.1: triethylamine / dmap / tert-butyl methyl ether / 2 h / 25 - 35 °C / Inert atmosphere
5.1: ethylaluminum dichloride / dichloromethane; toluene / 20 h / 0 - 35 °C / Inert atmosphere
5.2: Cooling
With
sulfuric acid; potassium tert-butylate; ethylaluminum dichloride; lithium tri-t-butoxyaluminum hydride; triethylamine;
dmap;
In
tetrahydrofuran; dichloromethane; tert-butyl methyl ether; toluene;
