Hydrochloric Acid → HCID 58277326、化合物
反応式
[Cl:1][C:2]1[CH:3]=[C:4]([N:9]2[C:13]([C:14]3[CH:19]=[C:18]([F:20])[CH:17]=[C:16]([Cl:21])[CH:15]=3)=[CH:12][C:11]([C:22]([O:24]CC)=[O:23])=[N:10]2)[CH:5]=[CH:6][C:7]=1[F:8].[OH-].[Li+].O.Cl>O1CCCC1>[Cl:1][C:2]1[CH:3]=[C:4]([N:9]2[C:13]([C:14]3[CH:19]=[C:18]([F:20])[CH:17]=[C:16]([Cl:21])[CH:15]=3)=[CH:12][C:11]([C:22]([OH:24])=[O:23])=[N:10]2)[CH:5]=[CH:6][C:7]=1[F:8]参加物
6
実験手順
5.11 g (12.9 mmol) of the compound of Example 21A are provided in 142 ml of tetrahydrofuran and, at room temperature, 3.08 g (129 mmol) of lithium hydroxide and 47 ml of water are added. The mixture is stirred at room temperature overnight and a 1N aqueous hydrogen chloride solution is subsequently added until the pH is acidic, the mixture extracted with ethyl acetate, and the organic phase is washed with water, dried over sodium sulfate, filtered and concentrated. 4.51 g (90% of theory) of the title compound are obtained.
後処理
- extractionthe mixture extracted with ethyl acetate
- washthe organic phase is washed with water
- dry with materialdried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-72873e60964743dea36c6b091c10f9be
- 出典データセット
- uspto-grants-2013_03
- 特許番号
- US08399682B2
反応ノート
読み込み中…