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HCID 15292629, Verbindung → HCID 131719743, Verbindung

HRID 1080632
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1080632
Cl.[NH2:2][CH2:3][CH2:4][O:5][NH2:6].[OH:7][C@H:8]1[CH2:25][CH2:24][C@@:23]2([CH3:26])[C@H:10]([CH2:11][CH2:12][C@@H:13]3[C@@H:22]2[CH2:21][CH2:20][C@@:18]2([CH3:19])[C@:14]3([OH:30])[CH2:15][CH2:16][C@@H:17]2[CH2:27][CH:28]=O)[CH2:9]1>[OH-].[Na+].O1CCOCC1>[NH2:2][CH2:3][CH2:4][O:5][N:6]=[CH:28][CH2:27][C@H:17]1[CH2:16][CH2:15][C@:14]2([OH:30])[C@H:13]3[C@H:22]([CH2:21][CH2:20][C@:18]12[CH3:19])[C@:23]1([CH3:26])[C@@H:10]([CH2:9][C@@H:8]([OH:7])[CH2:25][CH2:24]1)[CH2:11][CH2:12]3
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Komponenten

5

Edukt 2

HCID 15292629HCID 15292629, VerbindungHCID 233652242-(Aminooxy)ethanamine hydrochloride

Produkt 1

HCID 131719743HCID 131719743, VerbindungAusbeute 52,7 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 14798Sodium HydroxideLösungsmittelHCID 312751,4-DioxaneLösungsmittel2×

Versuchsvorschrift

To a solution of 0.47 g of 2-aminoethoxyamine hydrochloride in 16 ml of 1N NaOH and 20 ml of dioxane a solution of 0.89 g of 3β,14β-dihydroxy-5β-androstane-17β-ylacetaldehyde (Prepn. 2) in 15 ml of dioxane was added at room temperature. After 20 hrs the solution was extracted with ethyl acetate; the organic layer was dried over anhydrous sodium sulfate and evaporated to dryness. The crude product was purified by flash chromatography (SiO2) using chloroform with increasing amounts of methanol (6 to 20%) as the eluant. The fractions containing the title compound were collected and evaporated to dryness. The residue was ground with di-iso-propyl ether to give 0.55 g of the title compound (I-bf), as a white foam.

Aufarbeitung

  1. extractionAfter 20 hrs the solution was extracted with ethyl acetate
  2. dry with materialthe organic layer was dried over anhydrous sodium sulfate
  3. customevaporated to dryness
  4. customThe crude product was purified by flash chromatography (SiO2)
  5. additionThe fractions containing the title compound
  6. customwere collected
  7. customevaporated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-e3561d84c3754cf0943c1167493f7d35
Quelldatensatz
uspto-grants-1996_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05583127

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