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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Potassium Carbonate → HCID 21833755, 화합물

HRID 1741068
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HRID 1741068 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:13])[CH2:9][C:10](=O)[CH3:11])=[CH:4][C:3]=1[CH3:14].Cl.[NH2:16]O.C(=O)([O-])[O-].[K+].[K+]>C(O)C>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[O:13][N:16]=[C:10]([CH3:11])[CH:9]=2)=[CH:4][C:3]=1[CH3:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 21833711HCID 21833711, 화합물

생성물 1

HCID 21833755HCID 21833755, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 1-(4-bromo-3-methylphenyl)butane-1,3-dione (D77) (615 mg; 0.0024 ml) in ethanol (15 ml) was treated with hydroxylamine hydrochloride (170 mg; 0.0024 mol) and potassium carbonate (336 mg; 0.0024 mol), and the mixture heated at reflux for 2.5 hours, then overnight at room temperature. The solvent was evaporated under reduced pressure and the residue partitioned between water and ethyl acetate. The organic phase was dried (Na2SO4) and concentrated in vacuo to leave the crude isoxazole, which was purified by chromatography on silica gel, eluting with pentane, 60-80 petroleum-ether and ethyl acetate, to afford the title compound as a yellow crystalline material (477 mg, 78%).

후처리

  1. temperaturethe mixture heated
  2. temperatureat reflux for 2.5 hours
  3. customovernight
  4. customat room temperature
  5. customThe solvent was evaporated under reduced pressure
  6. customthe residue partitioned between water and ethyl acetate
  7. dry with materialThe organic phase was dried (Na2SO4)
  8. concentrationconcentrated in vacuo
  9. customto leave the crude isoxazole, which
  10. customwas purified by chromatography on silica gel
  11. washeluting with pentane, 60-80 petroleum-ether and ethyl acetate

출처 및 근거

ORD 기록
ord-b0f5f9c7670044a79c08f8b9efe952ed
출처 데이터셋
uspto-grants-1999_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05972951

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