Hydroxylamine → 2-Acetyl-4-(pyrid-2-yl)-pyrimidine oxime

HRID 933

反応式

HRID 933 の反応式
[C:1]([C:4]1[N:9]=[C:8]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][N:11]=2)[CH:7]=[CH:6][N:5]=1)(=O)[CH3:2].[NH2:16][OH:17].C([O-])(=O)C.[Na+]>C(O)C.O>[C:1](=[N:16][OH:17])([C:4]1[N:9]=[C:8]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][N:11]=2)[CH:7]=[CH:6][N:5]=1)[CH3:2]

参加物

6

反応物 3

HCID 787HydroxylamineHCID 517045Sodium AcetateHCID 196942132-Acetyl-4-(pyrid-2-yl)-pyrimidine

生成物 1

HCID 1363959922-Acetyl-4-(pyrid-2-yl)-pyrimidine oxime収率 91.1%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒2 回

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.

後処理

  1. temperaturewas heated
  2. temperatureto reflux for 1.5 hours
  3. filtrationfiltered
  4. washwashed with hexane

出典と根拠

ORDレコード
ord-25314cafe14044c4a971af24b93211f4
出典データセット
uspto-grants-1998_03
特許番号
US05723473

関連ノート

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