反应 #56537

ord-a743ed6fe47347c5aeb58ad11b43992b

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITIONis added dropwise at 10° C.
  2. 2
    温度heated on a steam bath for another 30 minutes
  3. 3
    其他The precipitate formed
  4. 4
    过滤is filtered
  5. 5
    洗涤the filtrate is washed with dilute hydrochloric acid, water, saturated sodium bicarbonate solution, saturated sodium chloride solution
  6. 6
    干燥dried over magnesium sulfate
  7. 7
    其他The solvent is evaporated
  8. 8
    其他to give 41.3 g

实验过程

To a mixture of 2-cyano-2-(2,4-dichlorophenyl)decan-1-ol (40 g., 0.12 mole) and methane sulfonyl chloride (15.3 g., 0.13 mole) in 2 liters of benzene is added dropwise at 10° C., 14.8 g., (0.14 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 41.3 g. of product, which is identified by nmr.

来源

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