반응 #5029

ord-ca2fd54a918b4c22a80531e0a6588ec9

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도After cooled
  2. 2
    여과The deposited crystal was collected by filtration
  3. 3
    세척washed with water
  4. 4
    기타dried

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05242912uspto-grants-1993_09