Ethyl 2-chloroacetoacetate → Ethyl 2-ethyl-4-methyl-1,3-thiazole-5-carboxylate
반응식
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]참가 물질
4
실험 절차
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.
후처리
- 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)
출처 및 근거
- ORD 기록
- ord-b83915895e264ac5ae4bcc8fa8f3e220
- 출처 데이터셋
- uspto-grants-2003_02
- 특허 번호
- US06515124B2
반응 노트
불러오는 중…