Technology Process of 1,3-dioxo-dodecahydro-6-phenylthio-2,2,8a-trimethyl-7(8H)-phenanthrenone
There total 5 articles about 1,3-dioxo-dodecahydro-6-phenylthio-2,2,8a-trimethyl-7(8H)-phenanthrenone which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
Multi-step reaction with 4 steps
1: 76 percent / 1 N L-selectride / tetrahydrofuran / 2 h / 1.) -78 deg C and -60 deg C, 2.) room temp.
2: 91 percent / lithium aluminium hydride / diethyl ether / 2 h / Heating
3: 1.) 5percent hydrochloric acid; 2.) p-toluenesulfonic acid monohydrate / 1.) water, THF, 3h, room temp.; 2.) heating, 2h
4: 1.) LDA, 2.) HMPA / 1.) THF, -78 deg C 30 min, room temp., 60 min; 2.) overnight, room temp.
With
hydrogenchloride; N,N,N,N,N,N-hexamethylphosphoric triamide; lithium aluminium tetrahydride; L-Selectride; toluene-4-sulfonic acid; lithium diisopropyl amide;
In
tetrahydrofuran; diethyl ether;
DOI:10.1016/S0040-4020(01)87396-8
- Guidance literature:
-
Multi-step reaction with 3 steps
1: 91 percent / lithium aluminium hydride / diethyl ether / 2 h / Heating
2: 1.) 5percent hydrochloric acid; 2.) p-toluenesulfonic acid monohydrate / 1.) water, THF, 3h, room temp.; 2.) heating, 2h
3: 1.) LDA, 2.) HMPA / 1.) THF, -78 deg C 30 min, room temp., 60 min; 2.) overnight, room temp.
With
hydrogenchloride; N,N,N,N,N,N-hexamethylphosphoric triamide; lithium aluminium tetrahydride; toluene-4-sulfonic acid; lithium diisopropyl amide;
In
diethyl ether;
DOI:10.1016/S0040-4020(01)87396-8
- Guidance literature:
-
Multi-step reaction with 5 steps
1: 75 percent / sodium methoxide / methanol / 2 h
2: 76 percent / 1 N L-selectride / tetrahydrofuran / 2 h / 1.) -78 deg C and -60 deg C, 2.) room temp.
3: 91 percent / lithium aluminium hydride / diethyl ether / 2 h / Heating
4: 1.) 5percent hydrochloric acid; 2.) p-toluenesulfonic acid monohydrate / 1.) water, THF, 3h, room temp.; 2.) heating, 2h
5: 1.) LDA, 2.) HMPA / 1.) THF, -78 deg C 30 min, room temp., 60 min; 2.) overnight, room temp.
With
hydrogenchloride; N,N,N,N,N,N-hexamethylphosphoric triamide; lithium aluminium tetrahydride; sodium methylate; L-Selectride; toluene-4-sulfonic acid; lithium diisopropyl amide;
In
tetrahydrofuran; methanol; diethyl ether;
DOI:10.1016/S0040-4020(01)87396-8
