反応 #74772

ord-4d1f016b8e124e3ba94a22611145c877

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度heated (80°-100° C.) for twenty-four hours
  2. 2
    その他The precipitated solid is collected
  3. 3
    洗浄washed well with water
  4. 4
    その他dried
  5. 5
    その他Recrystallization from cyclohexane yeilds material (19.75 g.) of m.p. 95°-97° C.

実験手順

Valeryl chloride (12.06 g., 0.10 mole) is added dropwise to a cooled stirred solution of 2-chloro-4-nitroaniline (17.26 g., 0.10 mole) in pyridine (100 ml.). The mixture is warmed to ambient temperature, 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 well with water and dried, 25.1 g., m.p. 80°-95° C. Recrystallization from cyclohexane yeilds material (19.75 g.) of m.p. 95°-97° C.

出典

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