Isoamyl Nitrite → Methyl 1,3-thiazole-5-carboxylate
반응식
N(OCCC(C)C)=O.[CH3:9][O:10][C:11]([C:13]1[S:17][C:16](N)=[N:15][CH:14]=1)=[O:12].C(OCC)(=O)C>O1CCOCC1>[CH3:9][O:10][C:11]([C:13]1[S:17][CH:16]=[N:15][CH:14]=1)=[O:12]참가 물질
5
반응 조건
- 온도
- 80 °C
실험 절차
The mixture of 2.15 g of isoamyl nitrite and 10 ml of dioxane was stirred at 80° C. under a nitrogen atmosphere. A solution of 1.23 g of 2-aminothiazole-5-carboxylic acid methyl ester (7-3) in 20 ml of dioxane was added drop wise. The mixture was refluxed for 2 hours. After cooling to room temperature 30 ml of ethyl acetate was added. The mixture was washed with brine and dried and the solvent evaporated under reduced pressure. The crude product is purified on silica, thus yielding 0.54 g (48%) of thiazol 5-carboxylic acid methyl ester (7-4).
후처리
- temperatureThe mixture was refluxed for 2 hours
- additionwas added
- washThe mixture was washed with brine
- customdried
- customthe solvent evaporated under reduced pressure
- customThe crude product is purified on silica
출처 및 근거
- ORD 기록
- ord-372d32bb21b14d429e50cd966c65ddb0
- 출처 데이터셋
- uspto-grants-2007_07
- 특허 번호
- US07244752B2
반응 노트
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