반응 #54293

ord-564ca0035b2b4a059e0434a65463c5bf

시약

없음

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타is brought to 120° C
  2. 2
    workup.WAITcontinued for 48 hours
  3. 3
    workup.ADDITIONthe mixture is poured into an 800 ml
  4. 4
    workup.STIRRINGice with stirring
  5. 5
    여과The mixture is filtered
  6. 6
    세척the solid washed extensively with water
  7. 7
    기타sucked dry
  8. 8
    기타dried in vacuo at 90°-95°

실험 절차

125 g. of 2,6 dimethyl aniline and 375 ml. of 88% formic acid are mixed in a 1 liter bomb with magnetic stirrer. The temperature (oil bath) is brought to 120° C. The bomb is kept at this temperature for 24 hours. The bomb is then allowed to cool to room temperature and stirring continued for 48 hours. The pressure is released and the mixture is poured into an 800 ml. ice with stirring. The mixture is filtered and the solid washed extensively with water and sucked dry and then dried in vacuo at 90°-95° to give N-formyl-2,6-dimethylaniline (m.p. 163°-164.5° C.).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04147804uspto-grants-1979_04