反应 #1824358

ord-68d96567e6804102b1ccf521cface524

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度was refluxed for 3 hours
  2. 2
    过滤filtered
  3. 3
    其他to remove the inorganic salts
  4. 4
    其他evaporated under vacuum
  5. 5
    workup.DISSOLUTIONThe crude product was dissolved in ether (100 mL)
  6. 6
    洗涤washed with H2O (2×20 mL) The organic layer
  7. 7
    干燥was dried (Na2SO4)
  8. 8
    其他evaporated
  9. 9
    其他to yield 4.5 g, 82.4% yield

实验过程

A mixture of 4'-hydroxy-3'-methylacetophenone (5.0 g, 33.3 mmol), iodomethane (5.7 g, 40.0 mmol), K2CO3 (granular, anhydrous) (23.0 g, 167 mmol), and acetone (250 mL) was refluxed for 3 hours. The reaction mixture was then cooled to room temperature, filtered to remove the inorganic salts, and evaporated under vacuum. The crude product was dissolved in ether (100 mL) and washed with H2O (2×20 mL) The organic layer was dried (Na2SO4) and evaporated to yield 4.5 g, 82.4% yield. The ketone was used in the following reaction without further purification.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05962314uspto-grants-1999_10