Water → HCID 22494336、化合物
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].O>C(O)C>[CH2:12]([C:11]1[S:14][C:8]([CH3:10])=[C:2]([C:3]([O:5][CH2:6][CH3:7])=[O:4])[N:15]=1)[CH3:13]参加物
5
実験手順
2.33 ml ethyl 2-chloroacetoacetate and 1.5 g thiopropionamide were dissolved in 30 ml ethanol, followed by stirring at room temperature for 16 hours. The reaction solution was ice-cooled and water was added thereto, followed by extracting with ethyl acetate. The organic layer was washed with brine, dried over anhydrous magnesium sulfate and evaporated. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=14:1), to give 0.8 g of ethyl 2-ethyl-5-methyl-1,3-thiazole-4-carboxylate.
後処理
- temperaturecooled
- extractionby extracting with ethyl acetate
- washThe organic layer was washed with brine
- dry with materialdried over anhydrous magnesium sulfate
- customevaporated
- customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=14:1)
出典と根拠
- ORDレコード
- ord-96d55e2770b54507ba34e6f8f0f7735e
- 出典データセット
- uspto-grants-2005_04
- 特許番号
- US06884821B1
反応ノート
読み込み中…