反応 #80282

ord-c317843f65ba47bebddd862b2745b9a7

反応条件

温度
70°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度was heated
  2. 2
    その他was returned to room temperature
  3. 3
    抽出extracted with ethyl acetate
  4. 4
    洗浄The organic layer was washed with water
  5. 5
    乾燥dried over anhydrous magnesium sulfate
  6. 6
    その他Crystals obtained by concentration under reduced pressure
  7. 7
    洗浄were washed with isopropyl ether

実験手順

A mixture comprising 54.2 g of 4-allyloxycarbonyl-5-hydroxy-2-methylbenzofuran-3-carboxylic acid, 47 g of 4,6-dimethoxy-2-methylsulfonylpyridine and 65 g of potassium carbonate in 200 ml of N,N-dimethylformamide, was heated and stirred at 70° C. for two hours. The mixture was returned to room temperature, and then the reaction solution was poured into water and extracted with ethyl acetate. The organic layer was washed with water and then dried over anhydrous magnesium sulfate. Crystals obtained by concentration under reduced pressure, were washed with isopropyl ether to obtain 79.2 g (yield: 98%) of the desired compound.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05616537uspto-grants-1997_04