反応 #57799

ord-f9885b2b86494950b21707d105682bc4

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONThe reaction mixture was added
  2. 2
    抽出the product was extracted with ether (3×50 mL)
  3. 3
    抽出The combined organic extract
  4. 4
    乾燥was dried over anhydrous Na2SO4 and ether
  5. 5
    その他was evaporated
  6. 6
    その他The product was purified by flash chromatography (silica-gel, 5-20% ethylacetate/hexane mobile phase)

実験手順

4-methyl-5-phenyl-oxazole (1.6 g, 10 mmol), prepared according to the literature (Heterocycles, 1977, 7, 77-80), was dissolved in chlorosulfonic acid (10 mL) and stirred at room temperature for 4 h. The reaction mixture was added to crushed ice (50 g) and the product was extracted with ether (3×50 mL). The combined organic extract was dried over anhydrous Na2SO4 and ether was evaporated. The product was purified by flash chromatography (silica-gel, 5-20% ethylacetate/hexane mobile phase) to yield 0.91 g of the desired-title compound light yellow solid. MS: m/z 258.0 (M++1).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07420055B2uspto-grants-2008_09