Reaktion #1101

Reaktionsgleichung

4-(1,4-dioxaspiro[4.5]dec-8-ylamino)-3-methoxy-2-methylpyridine hydrochloride

→

4-(4-Oxocyclohexylamino)-3-methoxy-2-methylpyridine hydrochloride

Lösungsmittel

formic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   Einengenafter concentrating in vacuo
2. 2
   workup.DISSOLUTIONis dissolved in methylene chloride
3. 3
   EinengenThe methylene chloride phase is concentrated
4. 4
   workup.DISSOLUTIONthe residue is dissolved in ether
5. 5
   Sonstigethe hydrochloride is precipitated by addition of ethereal HCl

Vorschrift

27.3 g of 4-(1,4-dioxaspiro[4.5]dec-8-ylamino)-3-methoxy-2-methylpyridine hydrochloride are stirred with 400 ml of formic acid for 4 hours. The residue which remains after concentrating in vacuo is dissolved in methylene chloride and shaken with 2N NaOH. The methylene chloride phase is concentrated, the residue is dissolved in ether and the hydrochloride is precipitated by addition of ethereal HCl. 14 g=90%; m.p.: 115° to 120° C.

Quelle