反応 #46725

ord-4ee9517eb9ec420cb4980422cdb446dd

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出extracted with diethylether (30 mL)
  2. 2
    乾燥The organic phase was dried (MgSO4)
  3. 3
    ろ過filtered
  4. 4
    その他the eluate evaporated

実験手順

To a solution of N-(2,4-dihydroxy phenyl)-2,2,2-trifluoro-acetamide (0.44 g; 2 mmol) in DMF (4 mL) was added K2CO3 and 1-bromooctane (0.37 mL; 2.1 mmol). The slurry was stirred for 2 days at room temperature, poured onto 0.1 M HCl (aq.; 50 mL) and then extracted with diethylether (30 mL). The organic phase was dried (MgSO4), filtered and the eluate evaporated to leave 550 mg of black solid which was purified by chromatography (SiO2; PE80-100° C./EtOAc=4:1) to leave 100 mg (15%) of a pure white solid. Mp. 114-116° C.; MS (GC-MS; Cl): 334 (MH+).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07741352B2uspto-grants-2010_06