反応 #80271

ord-b85621a70dcc4cf1a64757f4dd2df935

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 sodium sulfate
  6. 6
    濃縮Then, it was concentrated under reduced pressure
  7. 7
    その他the oily substance thereby obtained
  8. 8
    その他was purified by silica gel column chromatography (n-hexane/ethyl acetate=10/1)

実験手順

A mixture comprising 2.1 g of 4-formyl-5-hydroxy-3-methylbenzothiophene, 2.4 g of 4,6-dimethoxy-2-methylsulfonylpyrimidine and 1.8 g of potassium carbonate in 30 ml of N,N-dimethylformamide, was heated and stirred at 70° C. for 3 hours. The mixture was returned to room temperature, then poured into water and extracted with ethyl acetate. The organic layer was washed with water and then dried over anhydrous sodium sulfate. Then, it was concentrated under reduced pressure, and the oily substance thereby obtained was purified by silica gel column chromatography (n-hexane/ethyl acetate=10/1) to obtain 3.1 g (yield: 86%) of the desired compound.

出典

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