反应 #161155

ord-2027a42df18e4538b144b8a22b6323f4

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度was heated
  2. 2
    温度at reflux overnight
  3. 3
    温度After cooling
  4. 4
    其他The organic layer was separated
  5. 5
    萃取the aqueous phase was extracted with EtOAc (40×3 mL)
  6. 6
    洗涤The combined organic layers were washed with brine
  7. 7
    干燥dried over anhydrous Na2SO4
  8. 8
    浓缩concentrated under vacuum
  9. 9
    其他The residue was purified by column chromatography

实验过程

A mixture of N-[3-(3-methyl-but-3-enyloxy)-phenyl]-acetamide (2.5 g, 11.4 mmol) and AlCl3 (4.52 g, 34.3 mmol) in fluoro-benzene (50 mL) was heated at reflux overnight. After cooling, the reaction mixture was poured into water. The organic layer was separated and the aqueous phase was extracted with EtOAc (40×3 mL). The combined organic layers were washed with brine, dried over anhydrous Na2SO4 and concentrated under vacuum. The residue was purified by column chromatography to give N-(4,4-dimethyl-chroman-7-yl)-acetamide (1.35 g, 54%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08829204B2uspto-grants-2014_09