反応式
[N+:1]([C:4]1[CH:13]=[CH:12][C:7]([O:8][CH2:9][CH2:10][OH:11])=[CH:6][CH:5]=1)([O-])=O>CO.[Pd]>[NH2:1][C:4]1[CH:5]=[CH:6][C:7]([O:8][CH2:9][CH2:10][OH:11])=[CH:12][CH:13]=1参加物
4
実験手順
A solution of 2-(4-nitro-phenoxy)-ethanol (2.1 g, 12 mmol) in MeOH (30 mL) was flushed with argon and then charged with 10 wt % Pd/C (0.1 equiv by wt). The mixture was evacuated under house vacuum and then refilled with hydrogen from hydrogen balloon. The cycle was repeated again and the mixture stirred at room temperature for 2 h. The heterogeneous reaction mixture was filtered through a pad of Celite, washed with MeOH and concentrated in vacuo to furnish the title compound (1.8 g, 99%) as a brown solid. MS (ES+): m/z 154 (M+H)+.
後処理
- customThe mixture was evacuated under house vacuum
- additionrefilled with hydrogen from hydrogen balloon
- filtrationThe heterogeneous reaction mixture was filtered through a pad of Celite
- washwashed with MeOH
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-7dca8a8c9d3f47bb97f17ac105e26ac3
- 出典データセット
- uspto-grants-2009_05
- 特許番号
- US07528143B2
関連ノート
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