Réaction #1101

Équation de réaction

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

→

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

Solvants

formic acid

Conditions de réaction

Traitement

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

Mode opératoire

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.

Source