Reaktion #64131

Reaktionsgleichung

1,1-diethyl-3-[13-(1,3-dithiolan-2-yl)-2,6- dimethyl-8alpha-ergolinyl)-urea

→

1,1-Diethyl-3-(2,6,13-trimethyl-8alpha-ergolinyl)-urea

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   FiltrationIt is filtered by kieselguhr
2. 2
   Einengenthe solvent is concentrated by evaporation
3. 3
   Sonstigethe residue is chromatographed on silica gel with dichloromethane/methanol
4. 4
   Sonstigethe isolated substance is crystallized from methanol, yield 117 mg (31% of theory)

Vorschrift

458 mg of 1,1-diethyl-3-[13-(1,3-dithiolan-2-yl)-2,6- dimethyl-8alpha-ergolinyl)-urea (1 mmol) is dissolved in 50 ml of methanol and treated with several portions of Raney nickel at room temperature until the initial material has disappeared according to thin-layer chromatography. It is filtered by kieselguhr, the solvent is concentrated by evaporation and the residue is chromatographed on silica gel with dichloromethane/methanol, the isolated substance is crystallized from methanol, yield 117 mg (31% of theory).

Quelle