Réaction #5029

ord-ca2fd54a918b4c22a80531e0a6588ec9

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    TempératureAfter cooled
  2. 2
    FiltrationThe deposited crystal was collected by filtration
  3. 3
    Lavagewashed with water
  4. 4
    Autredried

Mode opératoire

7-Cyano-2,3,4,5-tetrahydro-1H-1-benzazepine-9-carboxylic acid benzyl ester (3.30 g) and sodium hydroxide (2 g) in a mixed solution of water-ethanol (1:1, 60 ml) was refluxed for 8 hours. After cooled, water (100 ml) was added to the reaction mixture, which was then rendered to have pH 3 with concentrated hydrochloric acid. The deposited crystal was collected by filtration, washed with water and dried to give the intended compound 1.84 g (85.0%), which was then recrystallized from ethanol to give slightly yellow crystal. M.P.: 287°-288° C.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US05242912uspto-grants-1993_09