Methyl 4-(3-hydroxyprop-1-ynyl)benzoate → Methyl 4-(3-hydroxypropyl)benzoate
反応式
[CH3:1][O:2][C:3](=[O:14])[C:4]1[CH:9]=[CH:8][C:7]([C:10]#[C:11][CH2:12][OH:13])=[CH:6][CH:5]=1>CCOC(C)=O.CO.[Pd]>[CH3:1][O:2][C:3](=[O:14])[C:4]1[CH:9]=[CH:8][C:7]([CH2:10][CH2:11][CH2:12][OH:13])=[CH:6][CH:5]=1参加物
5
実験手順
A solution of 4-(3-hydroxy-prop-1-ynyl)-benzoic acid methyl ester (12.65 g) in EtOAc (75 mL) and MeOH (75 mL) was hydrogenated at 50 psi on a Parr shaker in the presence of 10% palladium on carbon (2 g) for 24 h. The catalyst was removed by filtration through Celite® and the filtrate was concentrated. The reaction was repeated by adding 10% palladium on carbon (2 g) and hydrogenating on a Parr shaker for 24 h. After filtering through Celite®, the solution was concentrated in vacuo to provide 4-(3-hydroxy-propyl)-benzoic acid methyl ester (11.98 g).
後処理
- customThe catalyst was removed by filtration through Celite®
- concentrationthe filtrate was concentrated
- additionby adding 10% palladium on carbon (2 g)
- filtrationAfter filtering through Celite®
- concentrationthe solution was concentrated in vacuo
出典と根拠
- ORDレコード
- ord-b265b48860274e18a723be0ee3103e2e
- 出典データセット
- uspto-grants-2004_06
- 特許番号
- US06747054B2
反応ノート
読み込み中…