Technology Process of 1,2-Phenanthrenediol, 4b,5,6,7,8,8a,9,10-octahydro-4b,8,8-trimethyl-, (4bS,8aS)-
There total 16 articles about 1,2-Phenanthrenediol, 4b,5,6,7,8,8a,9,10-octahydro-4b,8,8-trimethyl-, (4bS,8aS)- which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
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Multi-step reaction with 9 steps
1: 1.) HNO3(d=1.52)-conc. H2SO4, 2.) conc. HCl, Sn dust / 1.) ice salt cooling, 2.) MeOH, 12 h, reflux
2: cc. H2SO4, NaNO3 / methanol / 0 - 5 °C
3: 2 h / Ambient temperature
4: 98 percent / H2 / 10 percent Pd-C, 60 percent HClO4 / ethyl acetate
5: 35 percent / HNO3(d=1.52) / acetic anhydride / 0.5 h / 0 - 4 °C
6: Sn dust, conc. HCl aq. / methanol / 12 h / Heating
7: 30 percent / (Me)3SiI / tetrahydrothiophene 1,1-dioxide / 3.5 h / 50 °C
8: NaIO4, 0.1 N HCl aq. / 0.13 h / Ambient temperature
9: KI / acetic acid; CHCl3 / 0.03 h
With
hydrogenchloride; tin; sodium nitrate; sodium periodate; trimethylsilyl iodide; sulfuric acid; hydrogen; nitric acid; potassium iodide;
palladium on activated charcoal; perchloric acid;
In
sulfolane; methanol; chloroform; acetic anhydride; acetic acid; ethyl acetate;
DOI:10.1248/cpb.29.1567
- Guidance literature:
-
Multi-step reaction with 8 steps
1: cc. H2SO4, NaNO3 / methanol / 0 - 5 °C
2: 2 h / Ambient temperature
3: 98 percent / H2 / 10 percent Pd-C, 60 percent HClO4 / ethyl acetate
4: 35 percent / HNO3(d=1.52) / acetic anhydride / 0.5 h / 0 - 4 °C
5: Sn dust, conc. HCl aq. / methanol / 12 h / Heating
6: 30 percent / (Me)3SiI / tetrahydrothiophene 1,1-dioxide / 3.5 h / 50 °C
7: NaIO4, 0.1 N HCl aq. / 0.13 h / Ambient temperature
8: KI / acetic acid; CHCl3 / 0.03 h
With
hydrogenchloride; tin; sodium nitrate; sodium periodate; trimethylsilyl iodide; sulfuric acid; hydrogen; nitric acid; potassium iodide;
palladium on activated charcoal; perchloric acid;
In
sulfolane; methanol; chloroform; acetic anhydride; acetic acid; ethyl acetate;
DOI:10.1248/cpb.29.1567