反応 #85793

ord-dd246b41c86a40e2bcd278fecf4bee3a

反応条件

温度
-5°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他the internal reaction temperature <10° C
  2. 2
    その他the reaction temperature below 0° C.
  3. 3
    その他of 40 minutes

実験手順

2,6-dichloropyridine-4-ylamine (10.0 g, 61 mmol) was slowly added in concentrated sulfuric acid (64 mL) at the rate to keep the internal reaction temperature <10° C. The mixture was then cooled to −5° C. and nitric acid (90%, 30 mL) was added dropwise to keep the reaction temperature below 0° C. over a period of 40 minutes. The reaction mixture was stirred at 0° C. for 2 hours and then poured into ice-water (500 mL). The title compound was isolated by filtration and dried in vacuo for the next step.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09434726B2uspto-grants-2016_09