Iodine → 3-tert-Butyl-1,2-thiazol-5-amine
反応式
[NH2:1]/[C:2](/[C:7]([CH3:10])([CH3:9])[CH3:8])=[CH:3]\[C:4](=[S:6])[NH2:5].C(=O)([O-])[O-].[K+].[K+].II.O>C(OCC)C>[C:7]([C:2]1[CH:3]=[C:4]([NH2:5])[S:6][N:1]=1)([CH3:10])([CH3:9])[CH3:8]参加物
6
実験手順
To a stirred solution of (Z)-3-amino-4,4-dimethyl-pent-2-enethioic acid amide (8.3 g, 525 mmol) and potassium carbonate (14.4 g, 105 mmol) in 140 mL of diethyl ether is added a solution of iodine (13.2 g, 52.5 mmol) in 20 mL of diethyl ether at reflux. The mixture is refluxed for 2 h and cooled. Water is added and the layers separated. The organic layer is washed with water, dried over sodium sulfate, filtered and concentrated under reduced pressure. The crude mixture is purified by flash chromatography to afford title compound in 53% yield. ESI m/z 157=MH+
後処理
- temperatureat reflux
- temperatureThe mixture is refluxed for 2 h
- temperaturecooled
- customthe layers separated
- washThe organic layer is washed with water
- dry with materialdried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customThe crude mixture is purified by flash chromatography
出典と根拠
- ORDレコード
- ord-645a3e4dff76486ea0323a44d40183d9
- 出典データセット
- uspto-grants-2014_01
- 特許番号
- US08629157B2
反応ノート
読み込み中…