Hydroxyamine hydrochloride → 6-Chloro-2-methylnicotinaldehyde oxime

HRID 386023ノート

反応式

HRID 386023 の反応式
[Cl:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=O)=[C:4]([CH3:10])[N:3]=1.Cl.[NH2:12][OH:13].C([O-])(=O)C.[Na+]>C(O)C>[Cl:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[N:12][OH:13])=[C:4]([CH3:10])[N:3]=1

参加物

5

反応物 3

HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 447548676-Chloro-2-methylpyridine-3-carbaldehyde

生成物 1

HCID 723159756-Chloro-2-methylnicotinaldehyde oxime

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

6-Chloro-2-methylnicotinaldehyde (1 g, 6.43 mmol), hydroxylamine hydrochloride (0.45 g, 6.43 mmol), and sodium acetate (0.53 g, 6.43 mmol) were dissolved in dry ethanol (32 ml) and transferred to a flame-dried round bottom flask. The reaction was allowed to stir at room temperature for 20 minutes. It was then concentrated under reduced pressure, re-dissolved in ethyl acetate, and washed with water. The aqueous layer was extracted with ethyl acetate two times. The organic layers were combined, dried over magnesium sulfate, filtered, and concentrated under reduced pressure. Purification was performed via silica gel chromatography (0-100% ethyl acetate in hexane) to afford the title compound.

後処理

  1. customtransferred to a flame-dried round bottom flask
  2. concentrationIt was then concentrated under reduced pressure
  3. dissolutionre-dissolved in ethyl acetate
  4. washwashed with water
  5. extractionThe aqueous layer was extracted with ethyl acetate two times
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure
  9. customPurification

出典と根拠

ORDレコード
ord-0c556354f091421a9426b2081ce36d16
出典データセット
uspto-grants-2013_02
特許番号
US08367706B2

反応ノート

読み込み中…