Methyl 4-chloroacetoacetate → HCID 22638557、化合物
反応式
[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]参加物
4
実験手順
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.
後処理
- 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)
出典と根拠
- ORDレコード
- ord-2014453ebfed4b299bfd8710bbe95500
- 出典データセット
- uspto-grants-2004_11
- 特許番号
- US06822097B1
反応ノート
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