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

HRID 1003969노트

반응식

HRID 1003969 반응식
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]

참가 물질

4

반응물 2

HCID 443297Hydroxyamine hydrochlorideHCID 18793911HCID 18793911, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-e89874c31ead44ebb9bf24e795d15ea6
출처 데이터셋
uspto-grants-2000_04
특허 번호
US06048852

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