Technology Process of tert-Butyl-[(2E,6E)-3,7-dimethyl-9-((1R,4aR,4bS,8aS,10aS)-2,4b,8,8,10a-pentamethyl-1,4,4a,4b,5,6,7,8,8a,9,10,10a-dodecahydro-phenanthren-1-yl)-nona-2,6-dienyloxy]-diphenyl-silane
There total 13 articles about tert-Butyl-[(2E,6E)-3,7-dimethyl-9-((1R,4aR,4bS,8aS,10aS)-2,4b,8,8,10a-pentamethyl-1,4,4a,4b,5,6,7,8,8a,9,10,10a-dodecahydro-phenanthren-1-yl)-nona-2,6-dienyloxy]-diphenyl-silane which
guide to synthetic route it.
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synthetic route:
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117638-20-7
(1S,4aR,4bS,8aS,10aR)-1-[(3E,7E)-9-(tert-Butyl-diphenyl-silanyloxy)-3,7-dimethyl-nona-3,7-dienyl]-2,4b,8,8,10a-pentamethyl-tetradecahydro-phenanthren-2-ol
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117638-15-0,139236-71-8,139236-72-9,145773-14-4
tert-Butyl-[(2E,6E)-3,7-dimethyl-9-((1R,4aR,4bS,8aS,10aS)-2,4b,8,8,10a-pentamethyl-1,4,4a,4b,5,6,7,8,8a,9,10,10a-dodecahydro-phenanthren-1-yl)-nona-2,6-dienyloxy]-diphenyl-silane
- Guidance literature:
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With
pyridine; thionyl chloride;
In
dichloromethane;
at -20 ℃;
for 1h;
DOI:10.1016/S0040-4039(00)96875-8
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117638-15-0,139236-71-8,139236-72-9,145773-14-4
tert-Butyl-[(2E,6E)-3,7-dimethyl-9-((1R,4aR,4bS,8aS,10aS)-2,4b,8,8,10a-pentamethyl-1,4,4a,4b,5,6,7,8,8a,9,10,10a-dodecahydro-phenanthren-1-yl)-nona-2,6-dienyloxy]-diphenyl-silane
- Guidance literature:
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Multi-step reaction with 7 steps
1: 99 percent / imidazole / dimethylformamide / 12 h / 23 °C
2: 1.) selenium dioxide, pyridine; 2.) sodium borohydride / 1.) ethanol, reflux, 1 h; 2.) ethanol, 0 deg C, 1 h
3: 68 percent / triphenylphosphine / CCl4 / 2 h / Heating
4: 81 percent / 1 h / -60 °C
5: 1.) titanium tetrachloride / 1.) methylene chloride, -78 deg C for 5 min, then up to 8 deg C; 2.) 8 deg C, 0.5 h
6: 93 percent / diethyl ether / 0 deg C 0.5 h and 23 deg C for 2 h
7: 82 percent / thionyl chloride, pyridine / CH2Cl2 / 1 h / -20 °C
With
pyridine; 1H-imidazole; sodium tetrahydroborate; selenium(IV) oxide; thionyl chloride; titanium tetrachloride; triphenylphosphine;
In
tetrachloromethane; diethyl ether; dichloromethane; N,N-dimethyl-formamide;
DOI:10.1016/S0040-4039(00)96875-8
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117638-15-0,139236-71-8,139236-72-9,145773-14-4
tert-Butyl-[(2E,6E)-3,7-dimethyl-9-((1R,4aR,4bS,8aS,10aS)-2,4b,8,8,10a-pentamethyl-1,4,4a,4b,5,6,7,8,8a,9,10,10a-dodecahydro-phenanthren-1-yl)-nona-2,6-dienyloxy]-diphenyl-silane
- Guidance literature:
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Multi-step reaction with 3 steps
1: 1.) titanium tetrachloride / 1.) methylene chloride, -78 deg C for 5 min, then up to 8 deg C; 2.) 8 deg C, 0.5 h
2: 93 percent / diethyl ether / 0 deg C 0.5 h and 23 deg C for 2 h
3: 82 percent / thionyl chloride, pyridine / CH2Cl2 / 1 h / -20 °C
With
pyridine; thionyl chloride; titanium tetrachloride;
In
diethyl ether; dichloromethane;
DOI:10.1016/S0040-4039(00)96875-8