Ethyl 2-chloroacetoacetate → Ethyl 2-ethyl-4-methyl-1,3-thiazole-5-carboxylate
反応式
Cl[CH:2]([C:8]([CH3:10])=O)[C:3]([O:5][CH2:6][CH3:7])=[O:4].[C:11]([NH2:15])(=[S:14])[CH2:12][CH3:13]>C(O)C>[CH2:6]([O:5][C:3]([C:2]1[S:14][C:11]([CH2:12][CH3:13])=[N:15][C:8]=1[CH3:10])=[O:4])[CH3:7]参加物
4
実験手順
A solution of ethyl 2-chloroacetoacetate (2.00 g, 10.04 mmol) and thiopropionamide (1.00 g, 11.22 mmol) in ethanol (100 mL) was heated at reflux overnight. The solvent was evaporated and dichloromethane (100 mL) added. The solution was washed with water (2×100 mL) and brine (100 mL), dried (MgSO4), filtered, evaporated and the concentrate was chromatographed over silica gel (10% ethyl acetate/hexanes) to give 2-ethyl-4-methylthiazole-5-carboxylic acid ethyl ester (1.63 g, 81% yield) as a colorless liquid.
後処理
- temperatureat reflux overnight
- customThe solvent was evaporated
- additiondichloromethane (100 mL) added
- washThe solution was washed with water (2×100 mL) and brine (100 mL)
- dry with materialdried (MgSO4)
- filtrationfiltered
- customevaporated
- customthe concentrate was chromatographed over silica gel (10% ethyl acetate/hexanes)
出典と根拠
- ORDレコード
- ord-b83915895e264ac5ae4bcc8fa8f3e220
- 出典データセット
- uspto-grants-2003_02
- 特許番号
- US06515124B2
反応ノート
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