Technology Process of (+/-)-2,3,6,7-tetrahydro-1-carbomethoxy-11β-(phenylthio)-16-methoxy-20,21-dinoraspidospermidin-8-one
There total 10 articles about (+/-)-2,3,6,7-tetrahydro-1-carbomethoxy-11β-(phenylthio)-16-methoxy-20,21-dinoraspidospermidin-8-one which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
In
toluene;
at 180 - 190 ℃;
for 24h;
in a sealed tube;
DOI:10.1021/ja00215a039
- Guidance literature:
-
Multi-step reaction with 8 steps
1: 95 percent / H2 / Raney-Ni / ethyl acetate / 18 h
2: 84 percent / POCl3 / 0.5 h / 0 °C
3: 79 percent / NaH / tetrahydrofuran / 0.25 h / from 0 deg C to room temp.
4: 100 percent / molecular sieves (3 Angstroem) / toluene / 23 h / 20 °C
5: 64 percent / diisopropylethylamine / toluene / 1 h / Heating
6: 98 percent / MCPBA, 10percent Na2CO3 / CH2Cl2; H2O / 1 h / 0 °C
7: 65 percent / 2,6-di-tert-butyl-4-methylpyridine, trifluoroacetic anhydride / toluene / 1 h / Heating
8: 88 percent / toluene / 24 h / 180 - 190 °C / in a sealed tube
With
2,6-di-tert-butyl-4-methylpyridine; 3 A molecular sieve; hydrogen; sodium hydride; sodium carbonate; N-ethyl-N,N-diisopropylamine; 3-chloro-benzenecarboperoxoic acid; trifluoroacetic anhydride; trichlorophosphate;
nickel;
In
tetrahydrofuran; dichloromethane; water; ethyl acetate; toluene;
DOI:10.1021/ja00215a039
- Guidance literature:
-
Multi-step reaction with 9 steps
1: 55 percent / 0.5M HCl, LiCl / CuCl / H2O; various solvent(s) / 5 deg C, 3.5 h. then 20 deg C, 4 h.
2: 95 percent / H2 / Raney-Ni / ethyl acetate / 18 h
3: 84 percent / POCl3 / 0.5 h / 0 °C
4: 79 percent / NaH / tetrahydrofuran / 0.25 h / from 0 deg C to room temp.
5: 100 percent / molecular sieves (3 Angstroem) / toluene / 23 h / 20 °C
6: 64 percent / diisopropylethylamine / toluene / 1 h / Heating
7: 98 percent / MCPBA, 10percent Na2CO3 / CH2Cl2; H2O / 1 h / 0 °C
8: 65 percent / 2,6-di-tert-butyl-4-methylpyridine, trifluoroacetic anhydride / toluene / 1 h / Heating
9: 88 percent / toluene / 24 h / 180 - 190 °C / in a sealed tube
With
hydrogenchloride; 2,6-di-tert-butyl-4-methylpyridine; 3 A molecular sieve; hydrogen; sodium hydride; sodium carbonate; N-ethyl-N,N-diisopropylamine; 3-chloro-benzenecarboperoxoic acid; trifluoroacetic anhydride; lithium chloride; trichlorophosphate;
nickel; copper(l) chloride;
In
tetrahydrofuran; dichloromethane; water; ethyl acetate; toluene;
DOI:10.1021/ja00215a039