Hydrochloric Acid → Ethyl 2-formyl-1,3-thiazole-4-carboxylate
反応式
C([O:3][CH:4](OCC)[C:5]1[S:6][CH:7]=[C:8]([C:10]([O:12][CH2:13][CH3:14])=[O:11])[N:9]=1)C.Cl>CC(C)=O>[CH:4]([C:5]1[S:6][CH:7]=[C:8]([C:10]([O:12][CH2:13][CH3:14])=[O:11])[N:9]=1)=[O:3]参加物
4
実験手順
Ethyl 2-(diethoxymethyl)-1,3-thiazole-4-carboxylate (1.34 g, 5.17 mmol; see step (iv) above) was taken up in acetone (100 mL) and a solution of 1N HCl (12.8 mL) was then added. The solution was refluxed for 45 min and the solvent removed under reduced pressure. The residue was then dissolved in ethyl acetate (40 mL) and extracted with saturated NaHCO3 solution (2×40 mL) and brine (2×40 mL). The organic fraction was then dried (MgSO4), filtered and the solvent removed under reduced pressure to yield the sub-title compound as a light brown solid (0.937 g, 98%).
後処理
- temperatureThe solution was refluxed for 45 min
- customthe solvent removed under reduced pressure
- dissolutionThe residue was then dissolved in ethyl acetate (40 mL)
- extractionextracted with saturated NaHCO3 solution (2×40 mL) and brine (2×40 mL)
- dry with materialThe organic fraction was then dried (MgSO4)
- filtrationfiltered
- customthe solvent removed under reduced pressure
出典と根拠
- ORDレコード
- ord-11a31948ecc140d4be71da7899c446b1
- 出典データセット
- uspto-grants-2011_09
- 特許番号
- US08012967B2
反応ノート
読み込み中…