Water → HCID 18177290, 화합물

HRID 337327

반응식

HRID 337327 반응식
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

참가 물질

6

반응물 4

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

생성물 1

HCID 18177290HCID 18177290, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-e9c81ae884da4740b800e223fd70c379
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08889727B2

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