Ethyl bromopyruvate → Imidazo[1,2-b][1,2,4]triazine-carboxylic acid ethyl ester
反応式
[NH2:1][C:2]1[N:3]=[N:4][CH:5]=[CH:6][N:7]=1.Br[CH2:9][C:10](=O)[C:11]([O:13][CH2:14][CH3:15])=[O:12]>C(O)C>[CH2:14]([O:13][C:11]([C:10]1[CH:9]=[N:1][C:2]2[N:4]([CH:5]=[CH:6][N:7]=2)[N:3]=1)=[O:12])[CH3:15]参加物
4
実験手順
A solution of 3-amino-1,2,4-triazine (5.0 g, 52 mmol) and ethyl bromopyruvate (11 mL, 88 mmol) in ethanol (50 mL) was heated to reflux for 20 minutes. The reaction was cooled to room temperature, and then partitioned between 200 mL of EtOAc and 200 mL of water. The layers were separated, and the organic layer was dried over MgSO4. The solids were removed by filtration, and then the solvent was removed by rotary evaporation. The residue was purified by chromatography (90 g SiO2, 50 to 70% EtOAc in hexanes) to give the desired product (181 mg, 1.8%). MS (ESI): 192.4 (M+H)+.
後処理
- temperatureto reflux for 20 minutes
- custompartitioned between 200 mL of EtOAc and 200 mL of water
- customThe layers were separated
- dry with materialthe organic layer was dried over MgSO4
- customThe solids were removed by filtration
- customthe solvent was removed by rotary evaporation
- customThe residue was purified by chromatography (90 g SiO2, 50 to 70% EtOAc in hexanes)
出典と根拠
- ORDレコード
- ord-b58162468cf648cfb6a71d2c4072f883
- 出典データセット
- uspto-grants-2006_12
- 特許番号
- US07151105B2
反応ノート
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