Potassium Carbonate → Ethyl 4-[(3-methoxyphenyl)sulfanyl]-3-oxobutanoate

HRID 490687노트

반응식

HRID 490687 반응식
Cl[CH2:2][C:3](=[O:10])[CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6].[CH3:11][O:12][C:13]1[CH:14]=[C:15]([SH:19])[CH:16]=[CH:17][CH:18]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[CH2:8]([O:7][C:5](=[O:6])[CH2:4][C:3](=[O:10])[CH2:2][S:19][C:15]1[CH:16]=[CH:17][CH:18]=[C:13]([O:12][CH3:11])[CH:14]=1)[CH3:9]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 69484Ethyl 4-chloroacetoacetateHCID 849893-Methoxybenzenethiol

생성물 1

HCID 21816283Ethyl 4-[(3-methoxyphenyl)sulfanyl]-3-oxobutanoate

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Ethyl 4-chloroacetoacetate (32.6 g, 0.188 mol), 3-methoxythiophenol (25.1 g, 0.179 mol) and DMF (700 mL) are combined and degassed by bubbling nitrogen through the stirred mixture for about 10 min, then potassium carbonate (50 g, 0.36 mol) is added to the stirred mixture in one batch. This mixture is stirred under nitrogen at room temperature for 2 h, the mixture is filtered to remove potassium carbonate, then diluted with ethyl acetate. The resulting solution is washed with water, then 5% aq. NaCl. The combined organics are washed with brine, dried over Na2SO4. Concentration yields the title compound as yellow liquid. This material is used without purification.

후처리

  1. customdegassed
  2. customby bubbling nitrogen through the stirred mixture for about 10 min
  3. filtrationthe mixture is filtered
  4. customto remove potassium carbonate
  5. additiondiluted with ethyl acetate
  6. washThe resulting solution is washed with water
  7. washThe combined organics are washed with brine
  8. dry with materialdried over Na2SO4
  9. concentrationConcentration

출처 및 근거

ORD 기록
ord-bb4f8852bb8d4c1f89a40ca8f7e0bf90
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07528160B2

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