Sodium Hydroxide → [(3,4,4-Trifluoro-3-butenyl)amino]oxoacetic acid
反応式
O=[C:2]([NH:9][C:10](=[O:15])[C:11]([O:13]C)=[O:12])[CH2:3][C:4]([F:8])=[C:5]([F:7])[F:6].[OH-].[Na+]>CO.O>[F:8][C:4](=[C:5]([F:6])[F:7])[CH2:3][CH2:2][NH:9][C:10](=[O:15])[C:11]([OH:13])=[O:12]参加物
5
実験手順
A solution of Compound 142 (3.16 g, 0.015 mole) in methanol (25 mL) is treated with a solution of NaOH (0.8 g, 0.02 mole) in water (5 mL). The solution is stirred at room temperature for 30 min and concentrated. The residue is dissolved in water (20 mL) and extracted with dichloromethane (2×30 mL). The aqueous layer is acidified with conc. HCl and extracted with ethyl acetate. The organic layer is dried and evaporated to give 0.75 g of the title compound as a white solid, a 25% yield. m.p. 95°-100° C.
後処理
- concentrationconcentrated
- dissolutionThe residue is dissolved in water (20 mL)
- extractionextracted with dichloromethane (2×30 mL)
- extractionextracted with ethyl acetate
- customThe organic layer is dried
- customevaporated
出典と根拠
- ORDレコード
- ord-3134fd599e064ef093bcefbff891ff83
- 出典データセット
- uspto-grants-1996_10
- 特許番号
- US05561162
反応ノート
読み込み中…