反应 #452180

ord-07b8d5e4910b4919b8045ec777fb6eeb

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度The resulting solution was refluxed for 2 hours
  2. 2
    workup.DISTILLATIONthe methanol was distilled off
  3. 3
    萃取extracted with chloroform

实验过程

Ammonium persulphate (102.7 g) in water (200 ml) was added over 40 minutes to a refluxing solution of 4-dimethylaminomethylpyridine (40.86 g), methanol (450 ml), water (210 ml) and concentrated sulphuric acid (30 ml). The resulting solution was refluxed for 2 hours, water (300 ml) was added and the methanol was distilled off. The cooled solution was basified and extracted with chloroform to give 4-dimethylaminomethyl-2-hydroxymethylpyridine (19.65 g) b.p. 92°-120°/0.06 mm Hg.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04607107uspto-grants-1986_08