반응 #42536

ord-4d6d13cf4e33436e8f7d59f215952097

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    세척washed with a saturated solution of NaHCO3, saturated NaCl
  2. 2
    건조dried (MgSO4)
  3. 3
    여과filtered
  4. 4
    농축concentrated under reduced pressure

실험 절차

A solution of 7-bromoisoquinolin-1-ol (2.5 g, 11.1 mmol) and POCl3 (10.4 mL, 111 mmol) was stirred at 70° C. for 2.5 h. The reaction mixture was cooled to room temperature, poured into ice water, and the solution was stirred overnight. The aqueous mixture was diluted with chloroform, washed with a saturated solution of NaHCO3, saturated NaCl, dried (MgSO4), filtered, and concentrated under reduced pressure to afford 7-bromo-1-chloroisoquinoline (2.3 g): 1H NMR (300 MHz, DMSO-d6) δ 8.39-8.36 (m, 2H), 8.09-8.02 (m, 2H), 7.95 (d, J=6 Hz, 1H).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07727997B2uspto-grants-2010_06