تفاعل #1101

معادلة التفاعل

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

→

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

المذيبات

formic acid

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.

المصدر