Hydroxyamine hydrochloride → 2-(1H-indene-1-yl)acetaldoxime

HRID 1534795ノート

反応式

HRID 1534795 の反応式
[CH:1]1([CH2:10][CH:11]=O)[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH:3]=[CH:2]1.Cl.[NH2:14][OH:15].C([O-])(=O)C.[Na+]>CO>[CH:1]1([CH2:10][CH:11]=[N:14][OH:15])[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH:3]=[CH:2]1

参加物

5

反応物 3

HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 19908307(1H-Inden-1-yl)acetaldehyde

生成物 1

HCID 856179012-(1H-indene-1-yl)acetaldoxime

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

2-(1H-indene-1-yl)acetaldehyde (1.5 g, 9.5 mmol), hydroxylamine hydrochloride (836 mg, 12.0 mmol), and sodium acetate (1.04 g, 12.7 mmol) were combined in methanol (50 ml) and stirred at ambient temperature overnight. The mixture was evaporated to dryness in vacuo and the residue treated with water and extracted with ether. The ether layer was washed with water, dried over sodium sulfate, filtered, and evaporated to dryness in vacuo. The residue was chromatographed on a silica gel coulmn eluted with 15% EtOAc in hexane followed by 22% EtOAc in hexane. The product fraction was evaporated to dryness in vacuo to provide 2-(1H-indene-1-yl)acetaldoxime.

後処理

  1. customThe mixture was evaporated to dryness in vacuo
  2. additionthe residue treated with water
  3. extractionextracted with ether
  4. washThe ether layer was washed with water
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. customevaporated to dryness in vacuo
  8. customThe residue was chromatographed on a silica gel
  9. washcoulmn eluted with 15% EtOAc in hexane
  10. customThe product fraction was evaporated to dryness in vacuo

出典と根拠

ORDレコード
ord-0af7707961c5422aa9463e46a4c489fc
出典データセット
uspto-grants-1992_02
特許番号
US05091387

反応ノート

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