반응 #85793

ord-dd246b41c86a40e2bcd278fecf4bee3a

반응 조건

온도
-5°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타the internal reaction temperature <10° C
  2. 2
    기타the reaction temperature below 0° C.
  3. 3
    기타of 40 minutes

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09434726B2uspto-grants-2016_09