反応 #707008

ord-a908043c8f7641fbb6ec451ab2193eb1

反応条件

温度
100°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度cooled
  2. 2
    その他The organic layer is separated
  3. 3
    洗浄washed with dilute NaOH and saturated NaCl
  4. 4
    乾燥dried (MgSO4)
  5. 5
    濃縮concentrated

実験手順

Bromophenol (3.74 g, 22 mmol) is stirred with 50% sodium hydroxide solution (16 mL) for about 1 hour then treated with hexadecyltributylphosphonium bromide (3.25 g, 6.4 mmol), 2.3-dichloro-pyridine (3.2 g, 21.6 mmol) and toluene (15 mL). The mixture is heated to 100° C. for 18 hours, cooled and diluted with ethyl acetate and water. The organic layer is separated, washed with dilute NaOH and saturated NaCl, dried (MgSO4) and concentrated. Flash chromatography (5% EtOAc/hexanes) yielded the title compound (4.4 g, 15 mmol).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05958918uspto-grants-1999_09