Reaktion #2374070

Reaktionsgleichung

xanthene-9-spiro-4'-tetrahydropyran-2'-one

methylamine

→

1'-methylxanthene-9-spiro-4'-piperidin-2'-one

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe gummy residue (0.52 g.) is chromatographed on silica gel
2. 2
   Wascheneluting
3. 3
   Temperaturwith increasing concentrations of chloroform in light petroleum (b.p. 60°-80° C.)
4. 4
   WaschenElution with 25% chloroform in light petroleum
5. 5
   Sonstigegives, on evaporation of the solvent
6. 6
   Sonstigea solid residue which is recrystallised from ethanol

Vorschrift

A mixture of xanthene-9-spiro-4'-tetrahydropyran-2'-one (0.5 g.) and methylamine (5 ml.) is heated at 250° C. for 4 hours in a steel bomb. The gummy residue (0.52 g.) is chromatographed on silica gel, eluting with increasing concentrations of chloroform in light petroleum (b.p. 60°-80° C.). Elution with 25% chloroform in light petroleum gives, on evaporation of the solvent, a solid residue which is recrystallised from ethanol to give 1'-methylxanthene-9-spiro-4'-piperidin-2'-one, m.p. 158°-159° C.

Quelle