Chloroacetic Acid → 1(2H)-Pyrazineacetic acid, 2-oxo-
反応式
[NH:1]1[CH:6]=[CH:5][N:4]=[CH:3][C:2]1=[O:7].[OH-].[Na+].Cl[CH2:11][C:12]([OH:14])=[O:13].Cl>>[O:7]=[C:2]1[CH:3]=[N:4][CH:5]=[CH:6][N:1]1[CH2:11][C:12]([OH:14])=[O:13]参加物
5
反応条件
- 温度
- 100 °C
実験手順
Pyrazin-2(1H)-one (0.333 g, 3.47 mmol) was added 5 N sodium hydroxide solution (2.1 mL) followed by chloroacetic acid (0.524 g, 5.54 mmol). The reaction mixture was heated at 100° C. for 2 h. After cooled down to ambient temperature, 2 N hydrochloric acid (3.5 mL) was added and the reaction mixture was directly purified by reverse phase HPLC (TMC Pro-Pac C18; 0-40% 0.1% trifluoroacetic acid in acetonitrile/0.1% trifluoroacetic acid in water gradient). The pure fractions were lyophilized overnight to yield the title compound as a yellow solid. LC/MS 155.2 (M+1).
後処理
- temperatureAfter cooled down to ambient temperature
- customthe reaction mixture was directly purified by reverse phase HPLC (TMC Pro-Pac C18; 0-40% 0.1% trifluoroacetic acid in acetonitrile/0.1% trifluoroacetic acid in water gradient)
出典と根拠
- ORDレコード
- ord-3cd525f9d558450cb86154a3b5790845
- 出典データセット
- uspto-grants-2012_08
- 特許番号
- US08247415B2
反応ノート
読み込み中…