Hydroxyamine hydrochloride → 2-Amino-pyridine-3-carbaldehyde oxime

HRID 77856

反応式

HRID 77856 の反応式
[NH2:1][C:2]1[C:7]([CH:8]=O)=[CH:6][CH:5]=[CH:4][N:3]=1.Cl.[NH2:11][OH:12]>N1C=CC=CC=1>[NH2:1][C:2]1[C:7]([CH:8]=[N:11][OH:12])=[CH:6][CH:5]=[CH:4][N:3]=1

参加物

4

反応物 2

HCID 443297Hydroxyamine hydrochlorideHCID 7376333-Pyridinecarboxaldehyde, 2-amino-

生成物 1

HCID 533951902-Amino-pyridine-3-carbaldehyde oxime収率 85%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To a solution of 2-amino-3-formylpyridine (1.00 g, 8.19 mmol) in pyridine (20 mL) was added hydroxylamine hydrochloride (854 mg, 12.3 mmol) at room temperature, which was stirred for 1 hour and 40 minutes at room temperature. The reaction solution was partitioned into water and ethyl acetate. The organic layer was washed with water and saturated aqueous sodium chloride, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under a reduced pressure. The residue was purified by NH silica gel column chromatography (ethyl acetate: methanol=10:1) to obtain the title compound (951 mg, 85%).

後処理

  1. customThe reaction solution was partitioned into water and ethyl acetate
  2. washThe organic layer was washed with water and saturated aqueous sodium chloride
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customthe solvent was evaporated under a reduced pressure
  5. customThe residue was purified by NH silica gel column chromatography (ethyl acetate: methanol=10:1)

出典と根拠

ORDレコード
ord-7d48683d5bce425bb760a1b931bcd747
出典データセット
uspto-grants-2014_09
特許番号
US08841327B2

関連ノート

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