반응 #82463

ord-617c5dc0849b4bb4b694c4bee7c154cd

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도the mixture is heated
  2. 2
    온도at reflux for 65 hours
  3. 3
    기타The triethyorthopropionate is removed in vacuo
  4. 4
    기타the resulting oil is purified by column chromatography
  5. 5
    workup.ADDITIONThe tractions containing the pure desired product

실험 절차

Diethyl 5-amino-1,6-dihydro-6-oxo-pyridine-2,3-dicarboxylate (7.57 g, 0.030 mol), is suspended in 60 mL triethylorthopropionate (TEOP 0.30 mol). A small amount of p-toluenesulfonic acid is added and the mixture is heated at reflux for 65 hours. The triethyorthopropionate is removed in vacuo and the resulting oil is purified by column chromatography. The tractions containing the pure desired product are combined and striped to a honey-colored oil weighing 7.38 g, yield 84.8%.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05622913uspto-grants-1997_04