反応 #1029

ord-25314cafe14044c4a971af24b93211f4

反応方程式

CC(=O)c1nccc(-c2ccccn2)n1
2-acetyl-4-(pyrid-2-yl)-pyrimidine
NO
hydroxylamine
CC(=O)[O-].[Na+]
sodium acetate
CC(=NO)c1nccc(-c2ccccn2)n1
2-acetyl-4-(pyrid-2-yl)-pyrimidine oxime
収率 91.1%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度was heated
  2. 2
    温度to reflux for 1.5 hours
  3. 3
    ろ過filtered
  4. 4
    洗浄washed with hexane

実験手順

A solution of 2-acetyl-4-(pyrid-2-yl)-pyrimidine (1.0 g), hydroxylamine (0.39 g) and sodium acetate (0.62 g) in a mixture of ethanol (10 ml) and water (2 ml) was heated to reflux for 1.5 hours. The reaction was then poured into water the precipitate filtered and washed with hexane to give 2-acetyl-4-(pyrid-2-yl)-pyrimidine oxime (0.98 g, 91% yield) as a white crystalline solid m.p. 196°-8° C.; 1H NMR: 2.50(3H,s); 7.42(1H,m); 7.88(1H,m); 8.30(1H,d); 8.59(1H,d); 8.74(1H,d); 8.90(1H,d); 10.85(1H,brs) ppm.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05723473uspto-grants-1998_03