تفاعل #74774

ord-a0b8289b302542d4a6f0f9aceaac2a49

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةthen heated (80°-100° C.) for twenty-four hours
  2. 2
    workup.STIRRINGwith stirring
  3. 3
    أخرىThe precipitated solid is collected
  4. 4
    غسيلwashed with water
  5. 5
    أخرىdried
  6. 6
    أخرىRecrystallization from butyl chloride
  7. 7
    أخرىprovides material of m.p. 115°-118° C.

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04173646uspto-grants-1979_11