반응 #88005

ord-28c544d32ed047e4b1cf1ee63257ed24

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도the resulting mixture was refluxed for 8 hours
  2. 2
    농축The solution was concentrated under vacuum
  3. 3
    workup.DISSOLUTIONthe crude was dissolved in DCM (150 ml)
  4. 4
    세척washed with 1N HCl (50 ml×2)
  5. 5
    건조the organic layer was dried over sodium sulfate
  6. 6
    기타the solvent was removed

실험 절차

To a solution of methyl 1-(4-nitrophenylsulfonyl)-1H-pyrrole-2-carboxylate (Int. 4) (550 mg, 1.773 mmol) in pyridine (25 ml), lithium iodide (1661 mg, 12.41 mmol) was added and the resulting mixture was refluxed for 8 hours. The solution was concentrated under vacuum and the crude was dissolved in DCM (150 ml) and washed with 1N HCl (50 ml×2) and then with brine (50 ml); the organic layer was dried over sodium sulfate and the solvent was removed affording 1-(4-nitrophenylsulfonyl)-1H-pyrrole-2-carboxylic acid (Int. 5) (433 mg, 1.462 mmol).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09440954B2uspto-grants-2016_09