反応 #1713029

ord-f87d05c106264f5b80bd27c31c67211e

反応条件

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

後処理

  1. 1
    その他The solvent was evaporated under reduced pressure
  2. 2
    workup.ADDITIONadded to the residue
  3. 3
    洗浄The mixture was washed successively with water and brine
  4. 4
    乾燥dried over sodium sulfate
  5. 5
    その他The solvent was evaporated under reduced pressure
  6. 6
    その他the residue was purified by silica gel column chromatography (hexane:ethyl acetate=100:0-90:10)

実験手順

A solution of thiazole (10.0 g), iodobenzene (2.63 ml), tetrakis(triphenylphosphine)palladium (0) (1.36 g) and potassium acetate (3.46 g) in N,N-dimethylacetamide (100 ml) was stirred under heating at 100° C. overnight. The solvent was evaporated under reduced pressure, and added to the residue was ethyl acetate. The mixture was washed successively with water and brine, and dried over sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (hexane:ethyl acetate=100:0-90:10) to give 5-phenylthiazole (1.50 g) as a pale yellow solid. APCI-Mass m/Z 162 (M+H).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08785403B2uspto-grants-2014_07