Ethyl (chloroformyl)acetate → Ethyl thiazole-5-carboxylate
반응식
[CH:1]([NH2:3])=[S:2].Cl[CH:5]([CH:11]=O)[C:6]([O:8][CH2:9][CH3:10])=[O:7]>CC(C)=O>[S:2]1[C:5]([C:6]([O:8][CH2:9][CH3:10])=[O:7])=[CH:11][N:3]=[CH:1]1참가 물질
4
실험 절차
To a round bottom flask was added 250 mL of dry acetone, 7.5 g (0.123 mol) of thioformamide, and 18.54 g (0.123 mol) of ethyl 2-chloro-2-formylacetate. The reaction was heated at reflux for 2 hours. The solvent was removed in vacuo, and the residue was purified by chromatography (SiO2, 6 cm o.d. column, 100% CHCl3, Rf =0.25) to provide 11.6 g (60%) of the desired compound as a light yellow oil. NMR (CDCl3) δ 1.39 (t, J=7 Hz, 3 H), 4.38 (q, J=7 Hz, 2 H), 8.50 (s, 1 H), 8.95 (s, 1 H).
후처리
- temperatureThe reaction was heated
- temperatureat reflux for 2 hours
- customThe solvent was removed in vacuo
- customthe residue was purified by chromatography (SiO2, 6 cm o.d
출처 및 근거
- ORD 기록
- ord-924bb5135ccf4469809c13ec0ee5f01c
- 출처 데이터셋
- uspto-grants-1997_04
- 특허 번호
- US05621109
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