反応式
C(O[C:4](=[O:14])[C:5]([C:8]1[CH:9]=[N:10][CH:11]=[CH:12][CH:13]=1)=[CH:6]O)C.[NH:15]([C:17]1[N:22]=[CH:21][CH:20]=[CH:19][N:18]=1)[NH2:16].[H-].[Na+].Cl>C(O)C>[N:10]1[CH:11]=[CH:12][CH:13]=[C:8]([C:5]2[C:4](=[O:14])[N:15]([C:17]3[N:22]=[CH:21][CH:20]=[CH:19][N:18]=3)[NH:16][CH:6]=2)[CH:9]=1参加物
6
実験手順
193 mg (1 mmol) of the compound from Example 2A and 116 mg (1.05 mmol) 2-hydrazinopyrimidine are initially introduced into 2 ml anhydrous ethanol under argon and the mixture is stirred at RT for 20 h. 40 mg (1 mmol) sodium hydride suspension (60% strength in paraffin oil) are then added in portions, a significant clouding of the reaction solution developing. The mixture is subsequently stirred at RT for 10 min. 1 ml 1 M hydrochloric acid is then added to the dark reaction mixture, a precipitate separating out. The precipitate is filtered off with suction and the residue is washed with water (2×1 ml) and dried in vacuo. 173 mg (72% of th.) of the title compound are obtained.
後処理
- stirringThe mixture is subsequently stirred at RT for 10 min
- customa precipitate separating out
- filtrationThe precipitate is filtered off with suction
- washthe residue is washed with water (2×1 ml)
- customdried in vacuo
出典と根拠
- ORDレコード
- ord-070ffdff072d47598df30111070eeaa4
- 出典データセット
- uspto-grants-2012_08
- 特許番号
- US08252817B2
関連ノート
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