Sodium Acetate → 4-Acetamidothiazole
반응식
[C:1]([NH:4][C:5]1[N:6]=[C:7](Br)[S:8][CH:9]=1)(=[O:3])[CH3:2].C([O-])(=O)C.[Na+].[H][H]>CO.[Pd]>[C:1]([NH:4][C:5]1[N:6]=[CH:7][S:8][CH:9]=1)(=[O:3])[CH3:2]참가 물질
6
실험 절차
A solution of 4-acetamido-2-bromo-thiazole (22 g., 0.2 m) and sodium acetate (8.2 g, 0.1 m) in methanol (600 ml) was hydrogenated at room temperature and 1 atm. pressure oven 10% palladium on carbon (5 g) until the theoretical uptake of hydrogen had occurred (about 3 hours). The catalyst was removed by filtration and the filtrate evaporated to dryness under reduced pressure. The residue was extracted with carbon tetrachloride (200 ml) in a Soxlet apparatus. The extract was cooled and the crystals removed by filtration to yield 4-acetamidothiazole (12 g, 78%). m.p. 176° C. Found: C, 41.8; H, 4.3; N, 19.3. C5H6N2OS requires: C, 42.2; H, 4.3; N, 19.7%.
후처리
- customwas hydrogenated at room temperature
- custom(about 3 hours)
- customThe catalyst was removed by filtration
- customthe filtrate evaporated to dryness under reduced pressure
- extractionThe residue was extracted with carbon tetrachloride (200 ml) in a Soxlet apparatus
- temperatureThe extract was cooled
- customthe crystals removed by filtration
출처 및 근거
- ORD 기록
- ord-046ef9b2bfec41d483dc686c5ab4e177
- 출처 데이터셋
- uspto-grants-1979_01
- 특허 번호
- US04134984
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