Technology Process of Pregna-1,4-diene-3,20-dione,9-fluoro-11,17-dihydroxy-21,21-diiodo-16-methyl-, (11b,16b)- (9CI)
There total 14 articles about Pregna-1,4-diene-3,20-dione,9-fluoro-11,17-dihydroxy-21,21-diiodo-16-methyl-, (11b,16b)- (9CI) which
guide to synthetic route it.
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synthetic route:
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37414-01-0
(8S,9R,10S,11S,13S,14S,16S,17R)-17-(2,2-Diiodo-acetyl)-9-fluoro-11,17-dihydroxy-10,13,16-trimethyl-6,7,8,9,10,11,12,13,14,15,16,17-dodecahydro-cyclopenta[a]phenanthren-3-one
- Guidance literature:
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With
iodine; calcium chloride; calcium oxide;
In
methanol;
at 25 - 27 ℃;
for 1h;
DOI:10.1080/00397910500464855
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37414-01-0
(8S,9R,10S,11S,13S,14S,16S,17R)-17-(2,2-Diiodo-acetyl)-9-fluoro-11,17-dihydroxy-10,13,16-trimethyl-6,7,8,9,10,11,12,13,14,15,16,17-dodecahydro-cyclopenta[a]phenanthren-3-one
- Guidance literature:
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Multi-step reaction with 7 steps
1.1: 95 percent / pyridine / 20 °C
2.1: 70 percent / triethyl orthoformate; p-toluenesulfonic acid / CH2Cl2 / 20 h / 20 °C
3.1: 72 percent / tetrahydrofuran; diethyl ether / 72 h / 60 °C
4.1: m-iodoxybenzoic acid; diphenyl diselenide / toluene / 22 h / Heating
4.2: 50 percent / p-toluenesulfonic acid / CH2Cl2 / 4 h / 20 °C
5.1: perchloric acid; 1,3-dibromo-5,5-dimethylhydantoin / dimethylformamide / 3 h / cooling
5.2: 75.8 percent / sodium hydroxide / CH2Cl2; methanol; H2O / 2 h / cooling
6.1: 80 percent / hydrofluoric acid / tetrahydrofuran; CH2Cl2 / 5 h / -70 - 0 °C
7.1: 100 percent / anhydrous calcium chloride; calcium oxide; iodine / methanol / 1 h / 25 - 27 °C
With
pyridine; perchloric acid; 1,3-dibromo-5,5-dimethylimidazolidine-2,4-dione; 3-iodosylbenzoic acid; diphenyl diselenide; hydrogen fluoride; iodine; toluene-4-sulfonic acid; orthoformic acid triethyl ester; calcium chloride; calcium oxide;
In
tetrahydrofuran; methanol; diethyl ether; dichloromethane; N,N-dimethyl-formamide; toluene;
DOI:10.1080/00397910500464855
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37414-01-0
(8S,9R,10S,11S,13S,14S,16S,17R)-17-(2,2-Diiodo-acetyl)-9-fluoro-11,17-dihydroxy-10,13,16-trimethyl-6,7,8,9,10,11,12,13,14,15,16,17-dodecahydro-cyclopenta[a]phenanthren-3-one
- Guidance literature:
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Multi-step reaction with 2 steps
1: 80 percent / hydrofluoric acid / tetrahydrofuran; CH2Cl2 / 5 h / -70 - 0 °C
2: 100 percent / anhydrous calcium chloride; calcium oxide; iodine / methanol / 1 h / 25 - 27 °C
With
hydrogen fluoride; iodine; calcium chloride; calcium oxide;
In
tetrahydrofuran; methanol; dichloromethane;
DOI:10.1080/00397910500464855