反応 #80288

ord-1f7760b0521044bf9540a7fb877206e6

反応条件

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The residue obtained by concentration under reduced pressure
  7. 7
    その他was crystallized from isopropyl ether

実験手順

A mixture comprising 2.2 g of benzyl 5-hydroxy-2-methylindol-4-carboxylate, 1.7 g of 4,6-dimethoxy-2-methylsulfonylpyrimidine and 1.3 g of potassium carbonate in 20 ml of N,N-dimethylformamide, was heated and stirred at a temperature of from 70° to 80° C. for two hours. The mixture was returned to room temperature, then poured into ice water and extracted with ethyl acetate. The organic layer was washed with water and then dried over anhydrous magnesium sulfate. The residue obtained by concentration under reduced pressure, was crystallized from isopropyl ether to obtain 2.8 g (yield: 85%) of the desired product. mp: 135°-139° C.

出典

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