反应 #46725

ord-4ee9517eb9ec420cb4980422cdb446dd

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    萃取extracted with diethylether (30 mL)
  2. 2
    干燥The organic phase was dried (MgSO4)
  3. 3
    过滤filtered
  4. 4
    其他the eluate evaporated

实验过程

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+).

来源

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