반응 #794529

ord-56a18bb87cc44d4a82b30b1f4dee6bd5

반응 조건

온도
180°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출extracted with ethyl acetate (2×50 mL)
  2. 2
    건조The organic layer was dried over sodium sulfate
  3. 3
    농축concentrated

실험 절차

A mixture of N1-(3-nitropyridin-2-yl)cyclohexane-1,4-diamine (500 mg, 2.11 mmol) and 2-chloro-1H-benzoimidazole (320 mg, 2.11 mmol) in N-methylpyrrolidinone (5 mL) was heated at 180° C. in microwave for 2 hours. The mixture was diluted with water (60 mL), and extracted with ethyl acetate (2×50 mL). The organic layer was dried over sodium sulfate and concentrated to give N1-(1H-benzo[d]imidazol-2-yl)-N4-(3-nitropyridin-2-yl)cyclohexane-1,4-diamine (400 mg, 1.13 mmol, 53.8% yield) which was used in the next step without further purification.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09174992B2uspto-grants-2015_11