反応 #74774

ord-a0b8289b302542d4a6f0f9aceaac2a49

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度then heated (80°-100° C.) for twenty-four hours
  2. 2
    workup.STIRRINGwith stirring
  3. 3
    その他The precipitated solid is collected
  4. 4
    洗浄washed with water
  5. 5
    その他dried
  6. 6
    その他Recrystallization from butyl chloride
  7. 7
    その他provides material of m.p. 115°-118° C.

実験手順

Valeryl chloride (12.06 g., 0.10 mole) is added dropwise to a cooled stirred solution of 4-nitroaniline (13.81 g., 0.10 mole) in pyridine (100 ml.). The resulting mixture is stirred at ambient temperature for one hour then heated (80°-100° C.) for twenty-four hours. The cooled solution is poured into cold 1 N hydrochloric acid (500 ml.) with stirring. The precipitated solid is collected, washed with water and dried, 21.4 g., m.p. 107°-116° C. Recrystallization from butyl chloride provides material of m.p. 115°-118° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04173646uspto-grants-1979_11