반응 #649754

ord-babd8341accc41f09964f38c2c0f1462

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타When the exothermic reaction
  2. 2
    workup.ADDITIONare added
  3. 3
    온도at reflux for 25 hours
  4. 4
    온도cooled to 0.degree
  5. 5
    여과and filtered
  6. 6
    세척Washing with 4.times
  7. 7
    건조100 ml of ethanol/diethyl ether (1:1) and drying

실험 절차

9.1 ml (0.13 mol) of 65% nitric acid are added dropwise in the course of 5 minutes to a yellow suspension of 20.0 g (0.13 mol) of 2-amino-4-nitrotoluene in 50 ml of absolute ethanol. When the exothermic reaction has subsided, 8.32 g (0.198 mol) of cyanamide dissolved in 8.3 ml of water are added. The brown reaction mixture is boiled at reflux for 25 hours, cooled to 0.degree. and filtered. Washing with 4.times.100 ml of ethanol/diethyl ether (1:1) and drying yield 2-methyl-5-nitrophenyl-guanidine nitrate; m.p. 219° C.-226° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08067421B2uspto-grants-2011_11