Chloroacetone → 1-(1-Phenyl-1H-pyrazol-5-yl)ethan-1-one

HRID 1747786노트

반응식

HRID 1747786 반응식
[C:1]1([NH:7][N:8]=[CH:9][CH:10]=O)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(=O)([O-])[O-].[K+].[K+].Cl[CH2:19][C:20](=[O:22])[CH3:21]>O1CCOCC1>[C:1]1([N:7]2[C:19]([C:20](=[O:22])[CH3:21])=[CH:10][CH:9]=[N:8]2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

참가 물질

5

반응물 3

HCID 6571ChloroacetoneHCID 11430Potassium CarbonateHCID 2774401(2-Phenylhydrazinylidene)acetaldehyde

생성물 1

HCID 534219791-(1-Phenyl-1H-pyrazol-5-yl)ethan-1-one수율 34.7%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

To a mixture of 2-(phenylhydrazono)ethanal (3.10 g) (Journal of Chemical Society, Perkin Trans. 1, 1981, 503-513.), potassium carbonate (4.40 g) and dioxane (20.0 mL) was added 1-chloropropan-2-one (2.10 g) at room temperature, and the mixture was heated under reflux for 5 hr. The reaction mixture was concentrated under reduced pressure and extracted with dichloromethane. The extract was washed with saturated brine, dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (dichloromethane/methanol) to give the title compound (1.35 g).

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 5 hr
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. extractionextracted with dichloromethane
  5. washThe extract was washed with saturated brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. customthe solvent was evaporated under reduced pressure
  8. customThe residue was purified by silica gel column chromatography (dichloromethane/methanol)

출처 및 근거

ORD 기록
ord-d83585c5f239434aa1cf5791c6808610
출처 데이터셋
uspto-grants-2015_10
특허 번호
US09150588B2

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