Technology Process of De-A,B-24-oxo-25-hydroxy-cholestan-8-benzyloxymethyl ether
There total 6 articles about De-A,B-24-oxo-25-hydroxy-cholestan-8-benzyloxymethyl ether which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
With
oxalyl dichloride; dimethyl sulfoxide; triethylamine;
In
dichloromethane;
at -78 - -10 ℃;
for 2.25h;
DOI:10.1016/S0039-128X(99)00110-5
- Guidance literature:
-
Multi-step reaction with 6 steps
1.1: 97 percent / Ph3P; imidazole; I2 / benzene / 3 h / 20 °C
2.1: 94 percent / dimethylformamide
3.1: 100 percent / Hunig's base / CH2Cl2 / 20 °C
4.1: diisopropylamine; tetramethylenediamine; n-BuLi / tetrahydrofuran; hexane / 0.25 h / -20 °C
4.2: 81 percent / tetrahydrofuran; hexane / 5 h
5.1: 86 percent / 5 percent Na/Hg; Na2HPO4 / methanol / 1 h / 0 °C
6.1: 71 percent / oxalyl chloride; DMSO; Et3N / CH2Cl2 / 2.25 h / -78 - -10 °C
With
1H-imidazole; disodium hydrogenphosphate; sodium amalgam; n-butyllithium; oxalyl dichloride; N,N,N,N,-tetramethylethylenediamine; iodine; dimethyl sulfoxide; triethylamine; diisopropylamine; N-ethyl-N,N-diisopropylamine; triphenylphosphine;
In
tetrahydrofuran; methanol; hexane; dichloromethane; N,N-dimethyl-formamide; benzene;
1.1: Iodination / 2.1: sulfonylation / 3.1: Etherification / 4.1: Metallation / 4.2: Ring cleavage / 5.1: Hydrogenolysis / 6.1: Oxidation;
DOI:10.1016/S0039-128X(99)00110-5
- Guidance literature:
-
Multi-step reaction with 5 steps
1.1: 94 percent / dimethylformamide
2.1: 100 percent / Hunig's base / CH2Cl2 / 20 °C
3.1: diisopropylamine; tetramethylenediamine; n-BuLi / tetrahydrofuran; hexane / 0.25 h / -20 °C
3.2: 81 percent / tetrahydrofuran; hexane / 5 h
4.1: 86 percent / 5 percent Na/Hg; Na2HPO4 / methanol / 1 h / 0 °C
5.1: 71 percent / oxalyl chloride; DMSO; Et3N / CH2Cl2 / 2.25 h / -78 - -10 °C
With
disodium hydrogenphosphate; sodium amalgam; n-butyllithium; oxalyl dichloride; N,N,N,N,-tetramethylethylenediamine; dimethyl sulfoxide; triethylamine; diisopropylamine; N-ethyl-N,N-diisopropylamine;
In
tetrahydrofuran; methanol; hexane; dichloromethane; N,N-dimethyl-formamide;
1.1: sulfonylation / 2.1: Etherification / 3.1: Metallation / 3.2: Ring cleavage / 4.1: Hydrogenolysis / 5.1: Oxidation;
DOI:10.1016/S0039-128X(99)00110-5
