反応式
[NH2:1][C:2]([NH2:4])=[O:3].C([O:7][C:8](=O)[CH:9]([F:15])[C:10](OCC)=[O:11])C.CC[O-].[Na+]>CCO>[F:15][C:9]1[C:8]([OH:7])=[N:1][C:2]([OH:3])=[N:4][C:10]=1[OH:11]参加物
5
実験手順
To a heterogeneous mixture of urea (641 mg, 10.67 mmol) and diethylfluoromalonate (1.96 g, 10.67 mmol) in EtOH (11 mL) was added 2.68 M NaOEt in EtOH (7.96 mL, 21.34 mmol). The mixture was heated at reflux for 60 h and then allowed to cool to room temperature. The mixture was filtered and the cake was then dissolved in warm water and the resulting solution was acidified with concentrated HCl to pH 2. The mixture was allowed to cool to room temperature and then cooled in an ice bath before filtering. The cake was washed with water and dried to afford 5-fluoropyrimidine-2,4,6-triol as a slightly off white solid (1.45 g, 93%).
後処理
- temperatureThe mixture was heated
- temperatureat reflux for 60 h
- filtrationThe mixture was filtered
- dissolutionthe cake was then dissolved in warm water
- temperatureto cool to room temperature
- temperaturecooled in an ice bath
- filtrationbefore filtering
- washThe cake was washed with water
- customdried
出典と根拠
- ORDレコード
- ord-705568b17178453dac59d6f41cc418a4
- 出典データセット
- uspto-grants-2014_02
- 特許番号
- US08653263B2
関連ノート
読み込み中…