Water → HCID 18177290、化合物

HRID 337327

反応式

HRID 337327 の反応式
Cl.[CH3:2][O:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[NH:10][NH2:11].[C:12]([CH2:15][C:16](=O)[CH3:17])(=O)[CH3:13].O.C(=O)([O-])[O-].[Na+].[Na+]>C(O)C>[CH3:2][O:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[N:10]1[C:16]([CH3:17])=[CH:15][C:12]([CH3:13])=[N:11]1

参加物

6

反応物 4

HCID 962WaterHCID 10340Sodium CarbonateHCID 31261AcetylacetoneHCID 28494452-Methoxyphenylhydrazine Hydrochloride

生成物 1

HCID 18177290HCID 18177290、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

3.50 g of 2-methoxyphenyl hydrazine hydrochloride was dissolved in 60 ml of ethanol, and 2.06 ml of acetyl acetone was added and heated at reflux for 1 hour. To the reaction mixture was added 150 ml of water, neutralized with saturated aqueous solution of sodium carbonate, and extracted with 150 ml of ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate, and then the solvent was distilled off under reduced pressure and purified by silica gel column chromatography (n-hexane:ethyl acetate=2:1) to yield 3.88 g of the title compound.

後処理

  1. temperatureheated
  2. temperatureat reflux for 1 hour
  3. extractionextracted with 150 ml of ethyl acetate
  4. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  5. distillationthe solvent was distilled off under reduced pressure
  6. custompurified by silica gel column chromatography (n-hexane:ethyl acetate=2:1)

出典と根拠

ORDレコード
ord-e9c81ae884da4740b800e223fd70c379
出典データセット
uspto-grants-2014_11
特許番号
US08889727B2

関連ノート

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