4-Bromophenol → 3-(4-Bromophenoxy)propan-1-ol
反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[CH:4][CH:3]=1.Br[CH2:10][CH2:11][CH2:12][OH:13].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH2:10][CH2:11][CH2:12][OH:13])=[CH:4][CH:3]=1参加物
5
実験手順
To a solution of 4-bromophenol (10 g, 58 mmol) in DMF (10 mL) was added 3-bromopropan-1-ol (9.6 g, 69 mmol) and potassium carbonate (13.6 g, 98 mmol). The mixture was stirred at room temperature for 12 h. LCMS showed the reaction was almost complete. The mixture was partitioned between water and ethyl acetate (20 mL×3), The combined organics were dried and concentrated to give the title compound that was used in the next step without further purification (14.7 g, quant). 1H NMR (400 MHz, CD3OD) δ 7.36 (d, 2H), 6.84 (d, 2H), 4.05 (t, 2H), 3.72 (t, 2H), 1.96 (m, 2H).
後処理
- customThe mixture was partitioned between water and ethyl acetate (20 mL×3)
- customThe combined organics were dried
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-7f54d6a6cb7b4c4b8b0c3ed45624452f
- 出典データセット
- uspto-grants-2014_11
- 特許番号
- US08889730B2
反応ノート
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