反応 #302853

ord-edcb51f8e09e40f495ada2de0721d14b

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The obtained mixture was reacted at room temperature for 30 minutes
  2. 2
    温度under cooling on ice
  3. 3
    ろ過The obtained precipitate was collected by filtration
  4. 4
    洗浄the filtrate was then washed with purified water

実験手順

5′-bromo-2′-hydroxyacetophenone (compound 12) (1.80 g, 10.6 mmol) was added to a pyridine solution (40 ml) that contained 4-methoxybenzoyl chloride (2.01 g, 9.35 mmol) in an ice bath. The obtained mixture was reacted at room temperature for 30 minutes, and the reaction solution was then poured into 1 N hydrochloric acid under cooling on ice. The obtained mixture was intensively stirred. The obtained precipitate was collected by filtration, and the filtrate was then washed with purified water, so as to obtain a product of interest, 4-methoxybenzoic acid 2-acetyl-4-bromophenyl ester (compound 13). Yield: 3.15 g (yield constant: 96.5%) 1H NMR (300 MHz, CDCl3) δ 7.72 (d, J=7.5 Hz, 1H), 8.06 (d, J=7.2 Hz, 1H), 8.86 (s, 1H), 10.13 (s, 1H).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08192717B2uspto-grants-2012_06