反应 #4078

ord-37aa6ea9a1e04e1a9edfeac185572691

反应条件

温度
95°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他equipped with stirrer, condenser
  2. 2
    温度thermometer, and heated
  3. 3
    温度Heating
  4. 4
    其他to rise to 115° C.
  5. 5
    workup.ADDITIONdropped, within 10 minutes, to 100° C
  6. 6
    温度With the application of heat
  7. 7
    温度a temperature of 90°-95° C. was maintained for 30 minutes

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04723040uspto-grants-1988_02