反応式
C(O[C:4](=[O:15])[CH2:5][C:6]([C:8]1[CH:13]=[C:12]([Cl:14])[CH:11]=[CH:10][N:9]=1)=O)C.Cl.[C:17]([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][N:21]=1)(=[NH:19])[NH2:18].[OH-].[Na+]>C(O)C>[Cl:14][C:12]1[CH:11]=[CH:10][N:9]=[C:8]([C:6]2[N:19]=[C:17]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][N:21]=3)[N:18]=[C:4]([OH:15])[CH:5]=2)[CH:13]=1参加物
5
実験手順
13.15 g (58 mmol) of 3-(4-chloropyrid-2-yl)-3-oxopropionic acid ethyl ester are dissolved in 400 ml of ethanol, and 9.10 g (58 mmol) of 2-amidinopyridine hydrochloride are added. After the addition of 14.44 ml of 4N sodium hydroxide solution, refluxing is carried out for 7 hours. The mixture is cooled and concentrated to a fifth of its original volume. The crude product is filtered off and recrystallised from methanol, yielding 6-(4-chloropyrid-2-yl)-2-pyrid-2-yl-pyrimidin-4-ol in the form of beige needles.
後処理
- temperaturerefluxing
- temperatureThe mixture is cooled
- concentrationconcentrated to a fifth of its original volume
- filtrationThe crude product is filtered off
- customrecrystallised from methanol
出典と根拠
- ORDレコード
- ord-50dd2ffd8b7a465cb271288798fa8a71
- 出典データセット
- uspto-grants-2007_11
- 特許番号
- US07291584B2
関連ノート
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