Tert-Butyl nitrite → Methyl 5-methyl-1,3-thiazole-4-carboxylate
反応式
N[C:2]1[S:3][C:4]([CH3:11])=[C:5]([C:7]([O:9][CH3:10])=[O:8])[N:6]=1.N(OC(C)(C)C)=O>O1CCCC1.O>[CH3:11][C:4]1[S:3][CH:2]=[N:6][C:5]=1[C:7]([O:9][CH3:10])=[O:8]参加物
5
反応条件
- 温度
- 50 °C
実験手順
To a solution of methyl 2-amino-5-methyl-1,3-thiazole-4-carboxylate (2.15 g, 12.5 mmol) in tetrahydrofuran (60 mL) was slowly added tert-butyl nitrite (2.23 mL, 18.7 mmol) with stirring at 50° C., and the mixture was stirred at 60° C. for 2 hr. The mixture was diluted with water (100 mL), and extracted with ethyl acetate (100 mL×2). The organic layer was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (hexane/ethyl acetate=80/20→0/100) to give the title compound (1.17 g, yield 60%).
後処理
- stirringthe mixture was stirred at 60° C. for 2 hr
- extractionextracted with ethyl acetate (100 mL×2)
- concentrationThe organic layer was concentrated under reduced pressure
- customthe residue was purified by silica gel column chromatography (hexane/ethyl acetate=80/20→0/100)
出典と根拠
- ORDレコード
- ord-02012051ffb148db8b7de8193bc052e3
- 出典データセット
- uspto-grants-2011_10
- 特許番号
- US08044049B2
反応ノート
読み込み中…