반응 #56387

ord-8cad7758f10c4a5abd3dddc305038682

반응 조건

온도
-10°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONTo this suspension are added
  2. 2
    기타at -10° C.
  3. 3
    workup.WAITto stand for a further 16 hours at room temperature
  4. 4
    세척after which it is washed with water (2×400 ml)
  5. 5
    건조dried over anhydrous sodium sulphate
  6. 6
    여과filtered
  7. 7
    기타The excess chlorobenzene is then removed by water jet vacuum distillation

실험 절차

133 g of cyanuric chloride are suspended in 720 ml of chlorobenzene and cooled to -10° C. To this suspension are added with stirring 50 ml of cyclopropylamine dropwise over a period of 25 minutes. Keeping the temperature at -10° C., 96 ml of aqueous sodium hydroxide (30% NaOH) are added dropwise. The reaction mixture is then stirred at -10° C. for 11/2 hours and allowed to stand for a further 16 hours at room temperature, after which it is washed with water (2×400 ml), dried over anhydrous sodium sulphate and filtered. The excess chlorobenzene is then removed by water jet vacuum distillation. 138 g of 2-cyclopropylamino-4,6-dichloro-s-triazine in the form of white crystals are obtained.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04225598uspto-grants-1980_09