反応 #323111

ord-6c4d012b6e334e0abb9af4a9c6210c07

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度the resulting solution is refluxed 17 hours
  2. 2
    その他The excess n-butylamine is removed under reduced pressure (20 mm)
  3. 3
    workup.DISSOLUTIONThe oil is dissolved in 6N hydrochloric acid (30 ml.)
  4. 4
    温度the solution is heated on a steam bath for 40 minutes
  5. 5
    workup.ADDITIONThe hot acidic solution is poured into a hot saturated aqueous sodium carbonate solution with nitrogen bubbling through it
  6. 6
    抽出The basic solution is extracted with chloroform
  7. 7
    乾燥The chloroform is dried over sodium sulfate
  8. 8
    濃縮concentrated

実験手順

To 4-(2,3-epoxypropoxy)benzaldehyde (8.9 gms., 0.05 m) is added n-butylamine (30 ml.) and the resulting solution is refluxed 17 hours. The excess n-butylamine is removed under reduced pressure (20 mm). The oil is dissolved in 6N hydrochloric acid (30 ml.) and the solution is heated on a steam bath for 40 minutes. The hot acidic solution is poured into a hot saturated aqueous sodium carbonate solution with nitrogen bubbling through it. The basic solution is extracted with chloroform. The chloroform is dried over sodium sulfate and concentrated to yield 4-(3-n-butylamino-2-hydroxypropoxy)benzaldehyde, as an oil.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04642311uspto-grants-1987_02