반응 #4078

ord-37aa6ea9a1e04e1a9edfeac185572691

반응 조건

온도
95°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타equipped with stirrer, condenser
  2. 2
    온도thermometer, and heated
  3. 3
    온도Heating
  4. 4
    기타to rise to 115° C.
  5. 5
    workup.ADDITIONdropped, within 10 minutes, to 100° C
  6. 6
    온도With the application of heat
  7. 7
    온도a temperature of 90°-95° C. was maintained for 30 minutes

실험 절차

51.0 g (0.25 mole) N-cyclohexyl-4-nitrosoaniline, 20.0 g (50%) NaOH and 135 g n-hexanol were charged to a 0.5 liter three-necked round bottom flask equipped with stirrer, condenser and thermometer, and heated while stirring to 95° C. until the development of an exotherm was observed. Heating was discontinued, the reaction temperature continued to rise to 115° C. and then dropped, within 10 minutes, to 100° C. With the application of heat, a temperature of 90°-95° C. was maintained for 30 minutes. The reaction mixture contained no unreacted nitroso compound. The yield of the product was 64 wt. %; m.p. 59°-61° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04723040uspto-grants-1988_02