Isoamyl Nitrite → Methyl 1,3-thiazole-5-carboxylate
反応式
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]参加物
5
反応条件
- 温度
- 80 °C
実験手順
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).
後処理
- 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
出典と根拠
- ORDレコード
- ord-372d32bb21b14d429e50cd966c65ddb0
- 出典データセット
- uspto-grants-2007_07
- 特許番号
- US07244752B2
反応ノート
読み込み中…