반응 #1101

반응 방정식

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

→

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

용매

formic acid

반응 조건

후처리

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

실험 절차

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.

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