反応 #65763

ord-5d06f69e1ef642a6812d39fef1df4759

反応条件

温度
100°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.DISTILLATIONAfter solvent was distilled off
  2. 2
    ろ過the resulting crystals were collected by filtration with ethanol
  3. 3
    workup.ADDITIONWater was added to the crystals
  4. 4
    ろ過followed by collection of the crystals by filtration

実験手順

To 210 mg of 3-amino-6-chloro-4,5-diethoxycarbonyl-2-(4-methoxyphenyl)pyridine was added 3 ml of hydrazine monohydrate, and the mixture was heated at 100° C. in a stream of nitrogen for 30 minutes. After solvent was distilled off, the resulting crystals were collected by filtration with ethanol. Water was added to the crystals, and the mixture was neutralized with 1N hydrochloric acid, followed by collection of the crystals by filtration.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05420275uspto-grants-1995_05