Tert-Butyl nitrite → Methyl 5-methyl-1,3-thiazole-4-carboxylate
反応式
N(OC(C)(C)C)=O.N[C:9]1[S:10][C:11]([CH3:18])=[C:12]([C:14]([O:16][CH3:17])=[O:15])[N:13]=1>O1CCOCC1>[CH3:18][C:11]1[S:10][CH:9]=[N:13][C:12]=1[C:14]([O:16][CH3:17])=[O:15]参加物
4
反応条件
- 温度
- 60 °C
実験手順
To a solution of tert-butyl nitrite (24 mL, 202 mmol) in 1,4-dioxane (180 mL) was added a mixture of methyl 2-amino-5-methyl-1,3-thiazole-4-carboxylate (6.83 g, 40.0 mmol) in 1,4-dioxane (70 mL). The solution was stirred at 60° C. for 1 hour. After cooling to room temperature, the solvent was evaporated. The crude oil was purified by flash chromatography (0-20% EtOAc/hexanes), affording methyl 5-methyl-1,3-thiazole-4-carboxylate (3.95 g, 63%). The product was used for the next step without any further purification.
後処理
- temperatureAfter cooling to room temperature
- customthe solvent was evaporated
- customThe crude oil was purified by flash chromatography (0-20% EtOAc/hexanes)
出典と根拠
- ORDレコード
- ord-2c5a002a63aa4a6985e4e47089a58ad7
- 出典データセット
- uspto-grants-2015_05
- 特許番号
- US09040538B2
反応ノート
読み込み中…