反応 #323111
ord-6c4d012b6e334e0abb9af4a9c6210c07
反応条件
詳細条件
See reaction.notes.procedure_details.
後処理
- 1温度the resulting solution is refluxed 17 hours
- 2その他The excess n-butylamine is removed under reduced pressure (20 mm)
- 3workup.DISSOLUTIONThe oil is dissolved in 6N hydrochloric acid (30 ml.)
- 4温度the solution is heated on a steam bath for 40 minutes
- 5workup.ADDITIONThe hot acidic solution is poured into a hot saturated aqueous sodium carbonate solution with nitrogen bubbling through it
- 6抽出The basic solution is extracted with chloroform
- 7乾燥The chloroform is dried over sodium sulfate
- 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.