2-Acetyl-3,5-dimethylpyrazine → 3,5-Dimethyl-2-(1-hydroximinoethyl)pyrazine

HRID 1780624ノート

反応式

HRID 1780624 の反応式
[C:1]([C:4]1[C:9]([CH3:10])=[N:8][C:7]([CH3:11])=[CH:6][N:5]=1)(=O)[CH3:2].Cl.[NH2:13][OH:14].O.O.O.C([O-])(=O)C.[Na+]>CO>[CH3:10][C:9]1[C:4]([C:1](=[N:13][OH:14])[CH3:2])=[N:5][CH:6]=[C:7]([CH3:11])[N:8]=1

参加物

5

反応物 3

HCID 1047212-Acetyl-3,5-dimethylpyrazineHCID 443297Hydroxyamine hydrochlorideHCID 23665404Sodium Acetate Trihydrate

生成物 1

HCID 1363411963,5-Dimethyl-2-(1-hydroximinoethyl)pyrazine収率 87.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

2-Acetyl-3,5-dimethylpyrazine (2.65 g), hydroxylamine hydrochloride (2.5 g) and sodium acetate trihydrate (3.5 g) were refluxed in methanol (50 ml) for 1 hour. The reaction mixture was concentrated, diluted with water (75 ml) and extracted with ethyl acetate. The combined extracts were dried and concentrated to give an oil which was triturated with ether and 60°-80° C. petrol to give 3,5-dimethyl-2-(1-hydroximinoethyl)pyrazine (2.54 g, 87% yield) as a white solid (m.p. 85°-89° C.) and as a 1:1 mixture of (E/Z) isomers.

後処理

  1. concentrationThe reaction mixture was concentrated
  2. additiondiluted with water (75 ml)
  3. extractionextracted with ethyl acetate
  4. customThe combined extracts were dried
  5. concentrationconcentrated
  6. customto give an oil which
  7. customwas triturated with ether and 60°-80° C. petrol

出典と根拠

ORDレコード
ord-17f8307bf4dc471eb1d6649f2b745312
出典データセット
uspto-grants-1997_05
特許番号
US05631253

反応ノート

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