Methane → 3-(3,4-dimethylphenyl)propanoic Acid
反応式
[CH3:1][C:2]1[CH:3]=[C:4]([CH:9]=[CH:10][C:11]([OH:13])=[O:12])[CH:5]=[CH:6][C:7]=1[CH3:8].C>[Pd].CO>[CH3:1][C:2]1[CH:3]=[C:4]([CH2:9][CH2:10][C:11]([OH:13])=[O:12])[CH:5]=[CH:6][C:7]=1[CH3:8]参加物
5
実験手順
A mixture of 3-(3,4-dimethyl-phenyl)-acrylic acid (19.269 g; 109.355 mmol) and 10% palladium over activated charcoal (1.920 g) was placed under nitrogen before MeOH (300 ml) was carefully added. The resulting suspension was placed under vacuum, then under hydrogen (1 atm), and the reaction mixture was vigorously stirred at rt for 4 h. The reaction mixture was filtered over a pad of celite, and concentrated under reduced pressure to give the expected product 3-(3,4-dimethyl-phenyl)-propionic acid as a grey solid which was further dried under HV (19.070 g; 98%). LC-MS: tR=0.85 min; [M+H]+: no ionisation.
後処理
- additionwas carefully added
- filtrationThe reaction mixture was filtered over a pad of celite
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-9bd7e4d5ab694ba59375853062330669
- 出典データセット
- uspto-grants-2012_05
- 特許番号
- US08188082B2
反応ノート
読み込み中…