Hydroxyamine hydrochloride → 5-Bromo-4-methyl-pyridine-2-carbaldehyde oxime

HRID 1027594ノート

反応式

HRID 1027594 の反応式
[Br:1][C:2]1[C:3]([CH3:10])=[CH:4][C:5]([CH:8]=O)=[N:6][CH:7]=1.Cl.[NH2:12][OH:13].C([O-])(=O)C.[Na+]>CCO.O>[Br:1][C:2]1[C:3]([CH3:10])=[CH:4][C:5]([CH:8]=[N:12][OH:13])=[N:6][CH:7]=1

参加物

6

反応物 3

HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 594745005-Bromo-4-methylpicolinaldehyde

生成物 1

HCID 1363413885-Bromo-4-methyl-pyridine-2-carbaldehyde oxime収率 66%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

To a solution of the compound obtained in Step B (3.1 g) in EtOH (47.5 ml) and water (23 ml) were added hydroxylamine hydrochloride (1.4 g) and sodium acetate (1.9 g). The reaction was stirred for 15 min at room temperature. The white solid was filtered off and the solution concentrated in vacuo to afford the crude title product (2.2 g, white solid), which was used directly for the next step. LCMS (Method F) 2.09 min, M+H 564/566.

後処理

  1. filtrationThe white solid was filtered off
  2. concentrationthe solution concentrated in vacuo

出典と根拠

ORDレコード
ord-81b2912c0bab483b8928743b60cccea6
出典データセット
uspto-grants-2014_05
特許番号
US08735362B2

反応ノート

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