Reaktion #564353

ord-5974a54b8de34cc1931a9ce2ebd93e8e

Reaktionsgleichung

N#Cc1ccc(C=O)s1
5-cyano-2-thiophene carboxaldehyde
O=C(O)CC(=O)O
malonic acid
O=C(O)CC(=O)O
malonic acid
N#Cc1ccc(C=CC(=O)O)s1
3-(5-Cyano-2-thiophenyl)-propenoic acid

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturunder reflux for 2 hours
  2. 2
    SonstigeThe solution was evaporated
  3. 3
    Sonstigeto give a pale solid which
  4. 4
    Waschenwas washed with water
  5. 5
    Sonstigedried

Vorschrift

A stirred solution of 5-cyano-2-thiophene carboxaldehyde (3.3 g) and malonic acid (2.5 g) in pyridine (35 ml) and piperidine (0.7 ml) was heated under reflux for 2 hours adding further malonic acid (1.3 g) after 1 hour. The solution was evaporated and the residue was stirred with M hydrochloric acid solution (100 ml) to give a pale solid which was washed with water and dried, m.p. ca 260° C. (subliming).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04886885uspto-grants-1989_12