反応 #56542

ord-f715f38f52c542d8a142be43670ec7b6

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度heated on a steam bath for another 30 minutes
  2. 2
    その他The precipitate formed
  3. 3
    ろ過is filtered
  4. 4
    洗浄the filtrate is washed with dilute hydrochloric acid, water, saturated sodium bicarbonate solution, saturated sodium chloride solution
  5. 5
    乾燥dried over magnesium sulfate
  6. 6
    その他The solvent is evaporated
  7. 7
    その他to give 22 g

実験手順

To a mixture of 2-cyano-2-(2-chlorophenyl)-2-(4-chlorophenyl)ethanol (18 g., 0.06 mole) and methane sulfonyl chloride (7.8 g., 0.07 mole) in 200 ml. of benzene is added dropwise at 10° C., 7.5 g. (0.08 mole) of triethylamine. The reaction mixture is stirred at room temperature for 30 minutes and then heated on a steam bath for another 30 minutes. The precipitate formed is filtered and the filtrate is washed with dilute hydrochloric acid, water, saturated sodium bicarbonate solution, saturated sodium chloride solution and dried over magnesium sulfate. The solvent is evaporated to give 22 g. of product; mp 124°-7° C., which is identified by nmr.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04225723uspto-grants-1980_09