Reaktion #74774

Reaktionsgleichung

Valeryl chloride

4-nitroaniline

hydrochloric acid

→

4'-Nitrovaleranilide

Lösungsmittel

pyridine

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthen heated (80°-100° C.) for twenty-four hours
2. 2
   workup.STIRRINGwith stirring
3. 3
   SonstigeThe precipitated solid is collected
4. 4
   Waschenwashed with water
5. 5
   Sonstigedried
6. 6
   SonstigeRecrystallization from butyl chloride
7. 7
   Sonstigeprovides material of m.p. 115°-118° C.

Vorschrift

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.

Quelle