Hydroxyamine hydrochloride → Methyl α-(hydroxyimino)-4-(1-methylethyl)benzeneacetate

HRID 1003969ノート

反応式

HRID 1003969 の反応式
Cl.[NH2:2][OH:3].O=[C:5]([C:10]1[CH:15]=[CH:14][C:13]([CH:16]([CH3:18])[CH3:17])=[CH:12][CH:11]=1)[C:6]([O:8][CH3:9])=[O:7]>CO>[OH:3][N:2]=[C:5]([C:10]1[CH:15]=[CH:14][C:13]([CH:16]([CH3:18])[CH3:17])=[CH:12][CH:11]=1)[C:6]([O:8][CH3:9])=[O:7]

参加物

4

反応物 2

HCID 443297Hydroxyamine hydrochlorideHCID 18793911HCID 18793911、化合物

生成物 1

HCID 73856943Methyl α-(hydroxyimino)-4-(1-methylethyl)benzeneacetate

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Hydroxylamine hydrochloride (0.87 g) was added to a stirred solution of the previously obtained mixture of methyl 2-oxo-2-(4-isopropyl-phenyl)acetate and methyl 4-isopropylphenyl acetate (1.29 g) in methanol (20 ml). When the solid had dissolved the mixture was left overnight. The solvent was evaporated and the residue partitioned between ethyl acetate and water, the organic phase was washed with water and brine, dried over magnesium sulphate and evaporated. The product (307 mg) was obtained by column chromatography of the residue using gradient elution (Kieselgel 3:1 to 1:1 hexane:ethyl acetate). νmax (CHCl3)/cm-1 3568, 3295 and 1738. δH (250 MHz, CDCl3), 1.28 (6H, d, J 6.87), 2.95 (1H, heptet, J 6.92), 3.88 (3H, s), 7.32 (2H, dd, J 1.81 and 6.47), 7.47 (2H, dd, J 1.83 and 6.65), 9.59 (1H, s).

後処理

  1. dissolutionWhen the solid had dissolved the mixture
  2. customThe solvent was evaporated
  3. customthe residue partitioned between ethyl acetate and water
  4. washthe organic phase was washed with water and brine
  5. dry with materialdried over magnesium sulphate
  6. customevaporated

出典と根拠

ORDレコード
ord-e89874c31ead44ebb9bf24e795d15ea6
出典データセット
uspto-grants-2000_04
特許番号
US06048852

反応ノート

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