反応 #2439648

ord-f82add84701b404ebaaddb4c33555360

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出The aqueous mixture was extracted with five, 200 mL portions of ethyl ether
  2. 2
    洗浄the combined extracts were washed with five, 150 mL portions of water
  3. 3
    洗浄wash
  4. 4
    乾燥After drying over magnesium sulfate, filtration and evaporation of the solvent 140.8 g of the desired product
  5. 5
    その他was obtained

実験手順

A mixture of 197.7 g of 3-bromo-N-(1,1-dimethylethyl)thiophene-2-sulfonamide, 195.9 g of cuprous cyanide and 500 mL of dimethylformamide was heated to 150° for two and one half hours at which time none of the bromothiophene remained as indicated by thin layer chromatography. The reaction was cooled to room temperature and poured into 1500 mL of 10% aqueous sodium cyanide. The aqueous mixture was extracted with five, 200 mL portions of ethyl ether and the combined extracts were washed with five, 150 mL portions of water followed by one, 200 mL aqueous sodium chloride wash. After drying over magnesium sulfate, filtration and evaporation of the solvent 140.8 g of the desired product was obtained.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04877440uspto-grants-1989_10