反応 #4305

ord-81ada1811183440c81eed8afb7279bd4

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The solvent was removed in vacuo
  2. 2
    その他the residue was partitioned between methylene chloride and dilute sodium hydroxide
  3. 3
    乾燥The methylene chloride solution was dried over magnesium sulfate
  4. 4
    workup.ADDITIONMethanol was added
  5. 5
    その他A white precipitate was collected
  6. 6
    その他to give 81.30 g (74.5%) of white, crystalline solid, m.p. 211°-213° C.

実験手順

A mixture of 71.90 g (0.352 mole) of 2-chloroethyl phenyl sulfone, 37.45 g (0.350 mole) of benzylamine and 60 ml of triethylamine in 800 ml of acetonitrile was stirred at room temperature for ≈64 hr. The solvent was removed in vacuo and the residue was partitioned between methylene chloride and dilute sodium hydroxide. The methylene chloride solution was dried over magnesium sulfate, and the volume was reduced in vacuo to 300 ml. Methanol was added followed by an excess of ethereal hydrogen chloride. A white precipitate was collected to give 81.30 g (74.5%) of white, crystalline solid, m.p. 211°-213° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04724235uspto-grants-1988_02