Water → HCID 9932026, Verbindung

HRID 2292494Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2292494
Cl([O-])=O.[Na+].[F:5][C:6]1[CH:34]=[CH:33][C:9]([C:10]([C@H:12]2[CH2:17][CH2:16][C@H:15]3[C@H:18]4[C@H:28]([CH2:29][CH2:30][C@:13]23[CH3:14])[C@:26]2([CH3:27])[C:21]([CH:22]=[C:23]([CH:31]=[O:32])[CH2:24][CH2:25]2)=[CH:20][CH2:19]4)=[O:11])=[CH:8][CH:7]=1.P([O-])([O-])([O-])=[O:36].[Na+].[Na+].[Na+].O>CC(=CC)C.C1COCC1.C(O)(=O)C.C(O)(C)(C)C>[F:5][C:6]1[CH:7]=[CH:8][C:9]([C:10]([C@H:12]2[CH2:17][CH2:16][C@H:15]3[C@H:18]4[C@H:28]([CH2:29][CH2:30][C@:13]23[CH3:14])[C@:26]2([CH3:27])[C:21]([CH:22]=[C:23]([C:31]([OH:36])=[O:32])[CH2:24][CH2:25]2)=[CH:20][CH2:19]4)=[O:11])=[CH:33][CH:34]=1

Komponenten

9

Edukt 4

HCID 962WaterHCID 24243Trisodium PhosphateHCID 23668197Sodium ChloriteHCID 54571409HCID 54571409, Verbindung

Produkt 1

HCID 9932026HCID 9932026, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 4

HCID 176Acetic AcidLösungsmittelHCID 6386tert-ButanolLösungsmittelHCID 8028TetrahydrofuranLösungsmittelHCID 105532-Methyl-2-buteneLösungsmittel

Versuchsvorschrift

Sodium chlorite is added to a mixture of 17β-(4-fluorobenzoyl)-androsta-3,5-diene-3-carboxaldehyde, sodium phosphate, monobasic monohydrate in 2-methyl-2-butene in THF, H2O, and t-butanol at RT. After 6 h acetic acid was added, then the aqueous layer is extracted with EtOAc, the combined organic extracts are dried (MgSO4), filtered, concentrated, and flash chromatographed to yield the title compound.

Aufarbeitung

  1. customat RT
  2. extractionthe aqueous layer is extracted with EtOAc
  3. dry with materialthe combined organic extracts are dried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customflash chromatographed

Quellen und Nachweise

ORD-Eintrag
ord-b2c1cb349a34487c93452157e22a20ca
Quelldatensatz
uspto-grants-1997_11
Patentnummer
US05683995

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