Sodium Hydroxide → 3-(4-Cyano-3-hydroxy-phenyl)-propionic acid
反応式
C([O:3][C:4](=[O:16])[CH2:5][CH2:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]#[N:14])=[C:9]([OH:15])[CH:8]=1)C.[OH-].[Na+]>C(O)C.O>[C:13]([C:10]1[CH:11]=[CH:12][C:7]([CH2:6][CH2:5][C:4]([OH:16])=[O:3])=[CH:8][C:9]=1[OH:15])#[N:14]参加物
5
実験手順
A solution of 3-(4-Cyano-3-hydroxy-phenyl)-propionic acid ethyl ester (2.2 g, 10 mmol) in ethanol (10 mL) and water (40 mL) was treated with aqueous sodium hydroxide solution (2.5 M, 44 mL) at room temperature overnight. The solvent was removed under vacuum and the residue was dissolved in water (150 mL). The pH of the aqueous solution was adjusted to 2–4 by the addition of 3N HCl (aqueous) and the precipitate was then filtered and washed with water to give the title compound as white solid (1.88 g, 0.98 mmol, 98.4% yield). ESMS m/z: 192 [M+H]+.
後処理
- customThe solvent was removed under vacuum
- dissolutionthe residue was dissolved in water (150 mL)
- additionThe pH of the aqueous solution was adjusted to 2–4 by the addition of 3N HCl (aqueous)
- filtrationthe precipitate was then filtered
- washwashed with water
出典と根拠
- ORDレコード
- ord-bc4df98abb674dae8f045995e3eb0883
- 出典データセット
- uspto-grants-2006_09
- 特許番号
- US07109238B2
反応ノート
読み込み中…