反応 #62570

ord-611285cd275a424f86977e849e6ea951

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    ろ過The white solid was filtered
  2. 2
    洗浄washed with water
  3. 3
    乾燥dried in vacuo over P2O5

実験手順

4-Iodoveratrole (26.0 g, 0.0985M) in acetic acid (25 ml) was treated with bromine (6.5 ml, 0.127M) in acetic acid (30 ml) and stirred at room temperature for one hour. The mixture was diluted with water (300 ml) and treated with sodium bisulfite to discharge the excess bromine. The white solid was filtered, washed with water and dried in vacuo over P2O5 to give 4-bromo-5-iodoveratrole (33.0 g, 95% yield) as a white solid, mp 98°-100° C. (literature: Baker et al., J. Chem. Soc. 3986 (1961), mp 102°-104° C.). NMR (CDCl3) δ 3.83 ppm (s, 6H, (2x) OCH3), 7.06 (s, 1H, ArH), 7.21 (s, 1H, ArH).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04761413uspto-grants-1988_08