Ethanol → Ethyl 2-(3-methylisoxazol-5-yl)acetate
反応式
[CH3:1][C:2]1[CH:6]=[C:5]([CH2:7][C:8]([OH:10])=[O:9])[O:4][N:3]=1.[CH3:11][CH2:12]O.OS(O)(=O)=O>>[CH3:1][C:2]1[CH:6]=[C:5]([CH2:7][C:8]([O:10][CH2:11][CH3:12])=[O:9])[O:4][N:3]=1参加物
4
実験手順
To a solution of 2-(3-methylisoxazol-5-yl)acetic acid (7.28 g, 51.6 mmol) in EtOH (200 mL, 3425 mmol) was added concentrated H2SO4 (0.30 mL, 5.63 mmol) at room temperature. After 48 h, the reaction mixture was concentrated in vacuo to give a dark brown oil. The crude ester was filtered over a plug of silica (50 g) and the product was eluted with 40% Et2O:60% Hexanes (400 mL). The filtrate was subsequently concentrated to give the product ethyl 2-(3-methylisoxazol-5-yl)acetate (8.50 g, 50.2 mmol, 97% yield) as a clear oil. LC/MS m/z 170 [M+H]+.
後処理
- concentrationthe reaction mixture was concentrated in vacuo
- customto give a dark brown oil
- filtrationThe crude ester was filtered over a plug of silica (50 g)
- washthe product was eluted with 40% Et2O
- concentrationThe filtrate was subsequently concentrated
出典と根拠
- ORDレコード
- ord-a6e7ca9cd3bf41e0b6101287b4fdc531
- 出典データセット
- uspto-grants-2014_08
- 特許番号
- US08796261B2
反応ノート
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