Реакция #1101

ord-87cd3f597261426bbf9068b66cd80964

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

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

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05723450uspto-grants-1998_03