Reaktion #790904

Reaktionsgleichung

product

1,1'-Dimethyl-3,3'-{[(estra-1,3,5(10)triene-3,17β-diyl)dioxy]dicarbonyl}dipyridinium diiodide

1-(phenylmethyl)-4-(aminocarbonyl)-1,2-dihydropyridine

→

1,17β-Bis{[(1-methyl-1,4-dihydropyridin-3-yl)carbonyl]oxy}estra-1,3,5(10)-triene

Lösungsmittel

methylene chloride

acetonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwas added
2. 2
   SonstigeRemoval of the solvent under reduced pressure
3. 3
   Sonstigeafforded a solid, which
4. 4
   Sonstigeremoved by filtration
5. 5
   SonstigeThe filtrate was chromatographed several times on a neutral alumina column
6. 6
   Sonstigeprepared with methylene chloride
7. 7
   SonstigePurification and evaporation of the solvent in vacuo
8. 8
   Sonstigegave a solid foam

Vorschrift

One gram (1.31 mmol) of the product of Example 71 was dissolved in 100 mL of dry acetonitrile. To that solution, which was flushed with nitrogen, 0.28 g (1.31 mmol) of 1-(phenylmethyl)-4-(aminocarbonyl)-1,2-dihydropyridine was added, and the reaction mixture was stirred at 0° C. for l hour. Removal of the solvent under reduced pressure afforded a solid, which was suspended in methylene chloride and removed by filtration. The filtrate was chromatographed several times on a neutral alumina column prepared with methylene chloride. Purification and evaporation of the solvent in vacuo gave a solid foam. The product had the formula ##STR106## as confirmed by UV, NMR and elemental analyses.

Quelle