反応式
[OH:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[CH:4][C:3]=1[C:9](=O)[CH3:10]>CO.[Pd]>[CH2:9]([C:3]1[CH:4]=[CH:5][C:6]([CH3:8])=[CH:7][C:2]=1[OH:1])[CH3:10]参加物
4
実験手順
A mixture of 1-(2-hydroxy-4-methyl-phenyl)-ethanone (5 g, 33.3 mmol) and 10 wt % Pd/C (2 g, Degussa type) in MeOH (50 mL) was stirred under a balloon of H2 for 24 hours. The reaction mixture was filtered through a pad of celite washing with EtOAc. The filtrate was concentrated to a clear oil (4.5 g, 99%). 1H NMR (400 MHz, CDCl3): δ 1.23 (t, J=7.6 Hz, 3H), 2.27 (s, 3H), 2.59 (q, J=7.6 Hz, 2H), 4.68 (s, 1H), 6.59 (s, 1H), 6.71 (d, J=7.7 Hz, 1H), 7.01 (d, J=7.7 Hz, 1H).
後処理
- filtrationThe reaction mixture was filtered through a pad of celite
- washwashing with EtOAc
- concentrationThe filtrate was concentrated to a clear oil (4.5 g, 99%)
出典と根拠
- ORDレコード
- ord-5c40fda8b53c4921941afd1b2abcbe54
- 出典データセット
- uspto-grants-2009_01
- 特許番号
- US07473790B2
関連ノート
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