Methyl 4-chloroacetoacetate → HCID 22638557, 화합물
반응식
[CH3:1][CH2:2][C:3]1[CH:4]=[C:5]([C:9]([NH2:11])=[S:10])[CH:6]=[CH:7][N:8]=1.Cl[CH2:13][C:14](=O)[CH2:15][C:16]([O:18][CH3:19])=[O:17]>CO>[CH2:2]([C:3]1[CH:4]=[C:5]([C:9]2[S:10][CH:13]=[C:14]([CH2:15][C:16]([O:18][CH3:19])=[O:17])[N:11]=2)[CH:6]=[CH:7][N:8]=1)[CH3:1]참가 물질
4
실험 절차
A mixture of ethionamide (Aldrich) (1.65 g, 10.0 mmol) and methyl 4-chloroacetoacetate (Fluka) (1.41 g, 10.0 mmol) in 50 mL of anhydrous MeOH was heated at reflux for 18 h. The solvent was evaporated to give an oily residue that was purified by chromatography (gradient elution: 10-50% EtOAc in hexanes) to afford the title compound as a light brown oil. MS m/z: 263 (M+1). Calc'd for C13H14N2O2S: 262.08.
후처리
- temperaturewas heated
- temperatureat reflux for 18 h
- customThe solvent was evaporated
- customto give an oily residue that
- customwas purified by chromatography (gradient elution: 10-50% EtOAc in hexanes)
출처 및 근거
- ORD 기록
- ord-2014453ebfed4b299bfd8710bbe95500
- 출처 데이터셋
- uspto-grants-2004_11
- 특허 번호
- US06822097B1
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