4-Methoxyphenol → 2-Bromo-4-methoxyphenol
反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([OH:9])=[CH:5][CH:4]=1.[Br:10]Br>CN(C=O)C>[Br:10][C:7]1[CH:8]=[C:3]([O:2][CH3:1])[CH:4]=[CH:5][C:6]=1[OH:9]参加物
4
実験手順
To a solution of 4methoxyphenol (13.00 g, 104.84 mmol) in DMF (50 mL) was added bromine (5.40 mL, 104.84 mmol) at 0° C. The reaction was allowed to warm room temperature. After stirring for 2 h the reaction was quenched with water and extracted with ethyl acetate (3×200 mL). The combined organic extracts were washed with brine and dried (Na2SO4). Removal of the solvent under reduced pressure gave 21.28 g of the crude title compound as a dark oil: 1H NMR (250 MHz, CDCl3) d 7.49 (b, 1H), 6.96 (d. 1H), 6.72-6.62 (m, 2H). 3.71 (s, 3H).
後処理
- customwas quenched with water
- extractionextracted with ethyl acetate (3×200 mL)
- washThe combined organic extracts were washed with brine
- dry with materialdried (Na2SO4)
- customRemoval of the solvent under reduced pressure
出典と根拠
- ORDレコード
- ord-3f437c1a4cb440f4a63ff666520773fb
- 出典データセット
- uspto-grants-2002_11
- 特許番号
- US06482956B2
反応ノート
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