Hydroxyamine hydrochloride → 5-Carboxyethyl-2,4-dimethoxy-4'-methoxybenzophenone oxime

HRID 893419ノート

反応式

HRID 893419 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[C:6]([C:11](=O)[C:12]2[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[CH:14][CH:13]=2)=[CH:5][C:4]=1[CH2:21][CH2:22][C:23]([OH:25])=[O:24].Cl.[NH2:27][OH:28].C([O-])(=O)C.[Na+]>C(O)C>[C:23]([CH2:22][CH2:21][C:4]1[C:3]([O:2][CH3:1])=[CH:8][C:7]([O:9][CH3:10])=[C:6]([CH:5]=1)[C:11](=[N:27][OH:28])[C:12]1[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[CH:14][CH:13]=1)([OH:25])=[O:24]

参加物

5

反応物 3

HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 144609963-[2,4-Dimethoxy-5-(4-methoxybenzoyl)phenyl]propionic acid

生成物 1

HCID 867459445-Carboxyethyl-2,4-dimethoxy-4'-methoxybenzophenone oxime

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

37 g of 3-[2,4-dimethoxy-5-(4-methoxybenzoyl)phenyl]propionic acid, 22.4 g of hydroxylamine hydrochloride and 21 g of sodium acetate (anhydrous) are added to 300 ml of absolute ethanol, and the mixture is refluxed with exclusion of moisture for 24 hours. Insolubles are removed by suction, the filtrate is concentrated, and water is added to the residue. The pH is then adjusted to 2 with 1N hydrochloric acid, and the mixture is extracted with ethyl acetate. The organic phase is washed with water, dried over magnesium sulfate and concentrated. The residue is recrystallized from ethyl acetate/hexane.

後処理

  1. temperaturethe mixture is refluxed with exclusion of moisture for 24 hours
  2. customInsolubles are removed by suction
  3. concentrationthe filtrate is concentrated
  4. additionwater is added to the residue
  5. extractionthe mixture is extracted with ethyl acetate
  6. washThe organic phase is washed with water
  7. dry with materialdried over magnesium sulfate
  8. concentrationconcentrated
  9. customThe residue is recrystallized from ethyl acetate/hexane

出典と根拠

ORDレコード
ord-0237181bebd849ebaf988bb108ec4ff4
出典データセット
uspto-grants-1992_06
特許番号
US05124478

反応ノート

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