Water → 4-Ethylbenzo[d]oxazol-5-amine
反応式
[CH2:1]([C:3]1[C:8]2[N:9]=[CH:10][O:11][C:7]=2[CH:6]=[CH:5][C:4]=1[NH:12]C(=O)C(F)(F)F)[CH3:2].O.C(=O)([O-])[O-].[K+].[K+].C(OCC)(=O)C>CO>[NH2:12][C:4]1[CH:5]=[CH:6][C:7]2[O:11][CH:10]=[N:9][C:8]=2[C:3]=1[CH2:1][CH3:2]参加物
6
反応条件
- 温度
- 90 °C
実験手順
A solution of 4-ethyl-5-trifluoroacetamidobenzoxazole (14.13 mmol) in a 20% mixture of water in methanol (20 mL) is treated with anhydrous potassium carbonate (56.52 mmol). A reflux condenser is attached and the mixture is heated to 90° C. with an oil bath for five hours. The mixture is cooled to room temperature and distributed between ethyl acetate (100 mL) and water (100 mL). The ethyl acetate layer is dried over magnesium sulfate and concentrated under reduced pressure to yield a black residue. This material is purified by chromatography (silica gel, 50% ethyl acetate/hexanes) to afford 5-amino-4-ethylbenzoxazole.
後処理
- customA reflux condenser is attached
- temperatureThe mixture is cooled to room temperature
- dry with materialThe ethyl acetate layer is dried over magnesium sulfate
- concentrationconcentrated under reduced pressure
- customto yield a black residue
- customThis material is purified by chromatography (silica gel, 50% ethyl acetate/hexanes)
出典と根拠
- ORDレコード
- ord-dd41e73abcee457db3f9e19b0346cdc1
- 出典データセット
- uspto-grants-2000_08
- 特許番号
- US06110952
反応ノート
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