반응 #169619

ord-1d70321a9b6d4c8d8f80406ccfd472d1

용매

반응 조건

온도
50°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도heated at 90° C. for 2 h
  2. 2
    기타The solvent was removed in vacuo and hydrochloric acid (1 N aqueous)
  3. 3
    workup.ADDITIONwas added until pH ˜2
  4. 4
    여과The beige solid was collected via filtration
  5. 5
    세척washed twice with water
  6. 6
    기타dried

실험 절차

To a solution of methyl 1-amino-4-bromo-2-naphthoate hydrobromide (2.00 g, 5.54 mmol) in 20 mL of THF was added sodium hydroxide (11.1 mL, 20% aqueous, 55.4 mmol). The mixture was stirred at 50° C. for 20 h, then heated at 90° C. for 2 h. The solvent was removed in vacuo and hydrochloric acid (1 N aqueous) was added until pH ˜2. The beige solid was collected via filtration, washed twice with water, and dried to provide 1-amino-4-bromo-2-naphthoic acid that gave a mass ion (ES+) of 266.0 (79Br) for [M+H]+.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08846702B2uspto-grants-2014_09