反応 #65483

ord-20e4c1800cc544f48aba3caf50071023

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度was refluxed for 24 hours
  2. 2
    ろ過400 ml of ethyl acetate, filtered
  3. 3
    抽出extracted with ethyl acetate
  4. 4
    その他After drying
  5. 5
    ろ過filtering
  6. 6
    その他were eliminated under reduced pressure at a temperature of about 60° C.

実験手順

A mixture of 1.5 g of the product of Example 1, 100 ml of dimethylformamide and 3 g of cuprous cyanide was refluxed for 24 hours and the reaction mixture was taken up in 400 ml of water and 400 ml of ethyl acetate, filtered and extracted with ethyl acetate. After drying and filtering, the solvents were eliminated under reduced pressure at a temperature of about 60° C. to obtain after chromatography on silica (essence G: 80/ethyl acetate: 20) 1.03 g of the expected product melting at 116° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05420138uspto-grants-1995_05