Technology Process of 22-Oxo-5α,8α-(4-phenyl-3,5-dioxo-1,2,4-triazolidine-1,2-diyl)-23,24-dinor-6-cholene-1α,3β-diyl diacetate
There total 11 articles about 22-Oxo-5α,8α-(4-phenyl-3,5-dioxo-1,2,4-triazolidine-1,2-diyl)-23,24-dinor-6-cholene-1α,3β-diyl diacetate which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
With
pyridine;
In
dichloromethane;
at -65 ℃;
for 4.5h;
DOI:10.1246/bcsj.62.3132
- Guidance literature:
-
Multi-step reaction with 8 steps
1: t-BuOK / tetrahydrofuran / 33 h / Ambient temperature
2: 4-(dimethylamino)pyridine, pyridine / 0.75 h / Ambient temperature
3: 80 percent / boron trifluoride etherate / CH2Cl2 / 1 h / Ambient temperature
4: 98 percent / H2 / 5percent Pt/C / ethanol / Ambient temperature
5: N-bromosuccinimide / CCl4 / 0.25 h / Heating
6: 1.) n-Bu4NBr, 2.) n-Bu4NF / 1.) THF, r.t., 1 h, 2.) hexane, r.t., 45 min
7: ethyl acetate
8: 1.) DMSO, oxalyl chloride, 2.) Et3N / 1.) CH2Cl2, -78 deg C, 15 min, 2.) to r.t., 50 min
With
pyridine; dmap; N-Bromosuccinimide; oxalyl dichloride; boron trifluoride diethyl etherate; potassium tert-butylate; tetrabutyl ammonium fluoride; tetrabutylammomium bromide; hydrogen; dimethyl sulfoxide; triethylamine;
platinum on activated charcoal;
In
tetrahydrofuran; tetrachloromethane; ethanol; dichloromethane; ethyl acetate;
DOI:10.1021/jo00027a010
- Guidance literature:
-
Multi-step reaction with 7 steps
1: 4-(dimethylamino)pyridine, pyridine / 0.75 h / Ambient temperature
2: 80 percent / boron trifluoride etherate / CH2Cl2 / 1 h / Ambient temperature
3: 98 percent / H2 / 5percent Pt/C / ethanol / Ambient temperature
4: N-bromosuccinimide / CCl4 / 0.25 h / Heating
5: 1.) n-Bu4NBr, 2.) n-Bu4NF / 1.) THF, r.t., 1 h, 2.) hexane, r.t., 45 min
6: ethyl acetate
7: 1.) DMSO, oxalyl chloride, 2.) Et3N / 1.) CH2Cl2, -78 deg C, 15 min, 2.) to r.t., 50 min
With
pyridine; dmap; N-Bromosuccinimide; oxalyl dichloride; boron trifluoride diethyl etherate; tetrabutyl ammonium fluoride; tetrabutylammomium bromide; hydrogen; dimethyl sulfoxide; triethylamine;
platinum on activated charcoal;
In
tetrachloromethane; ethanol; dichloromethane; ethyl acetate;
DOI:10.1021/jo00027a010