반응 #65755

ord-85212bf9fa35470e9ef24fe3284c0ef7

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONwas added
  2. 2
    workup.DISTILLATIONAfter the solvent was distilled off
  3. 3
    추출followed by extraction with ethyl acetate
  4. 4
    세척The organic layer was washed with a saturated aqueous solution of sodium chloride
  5. 5
    기타dried
  6. 6
    workup.DISTILLATIONThe solvent was distilled off
  7. 7
    기타to give an oily product

실험 절차

In 15 ml of ethanol was dissolved 1.2 g of 2-chloro-3,4-diethoxycarbonyl-6-methyl-5-nitropyridine, whereto 1.9 g (9 eq.) of reduced iron was added, followed by adding dropwise 7.1 ml of hydrochloric acid. The mixture was stirred at room temperature for 30 minutes. After the solvent was distilled off, the residue was neutralized with sodium hydrogencarbonate, followed by extraction with ethyl acetate. The organic layer was washed with a saturated aqueous solution of sodium chloride and dried. The solvent was distilled off to give an oily product.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05420275uspto-grants-1995_05